gaba to gbl pdf

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(1)Modified GABA to GBL conversion and extraction Rev 4 By Cleaver, February 2005 Original chemistry and methodology by Chromic. GENERAL DISCLAIMER: I take no responsibility for ANY harm that may (and probably will) come to you by performing the steps outlined in this document. The steps in this document involve some of the most poisonous, reactive, and cancerous substances you can legally buy. If you do not understand the risk you are taking by attempting to follow my notes, please do not even try. I also make no claims whatsoever that the end result will be as stated in this document. I assume no liability WHATSOEVER for loss of equipment or damage to personal property if you should attempt these procedures..

(2) Introduction: ........................................................................................................................ 3 Reagents and quantities:...................................................................................................... 4 Suggested equipment........................................................................................................... 6 Step 1: Sandmeyer Reaction ............................................................................................. 12 1.1 Prepare your solution .............................................................................................. 12 1.2 prepare your acid..................................................................................................... 13 1.3 Assemble your dripping apparatus.......................................................................... 13 1.4 Begin dripping......................................................................................................... 15 Step 2: DCM extraction..................................................................................................... 16 Step 3: DCM Distillation .................................................................................................. 19 Step 4: GBL Distillation.................................................................................................... 21 Vacuum distillation ....................................................................................................... 21 Step 5: GBL to GHB conversion (simple method) ........................................................... 22 5.1 Calculate the amount of baking soda and water required ....................................... 23 Find the FW (formula weight) of your GBL solution............................................... 23 Find the rough amount of distilled water necessary.................................................. 23 Total .......................................................................................................................... 23 Theoretical GHB end-product................................................................................... 24 5.2 Prep the Baking Soda, water solution ..................................................................... 24 5.3 Reflux ...................................................................................................................... 24 5.4 Adjust PH ................................................................................................................ 24 5.5 Clarify...................................................................................................................... 24 5.6 (Optional) Distill water and crystallize ................................................................... 25 Quick calculations for various reagent quantities ............................................................. 26.

(3) Introduction: I have performed the GABA to GBL conversion several times using this method and it works very nicely for me. MANY thanks to Chromic for the initial conversion process documentation. Please observe two critical operations when performing this experiment: 1) Slow, careful HCL drip during Sandmeyer reaction. This is CRITICAL. If brown NO2 gas is forming at a significant rate, you are miss-treating a valuable reagent and, consequently the final yield. 2) DCM extraction: Take your time and swirl/shake the hell out of the DCM/solution mixture. Allow enough time to let the GBL migrate out of the solution into the DCM. Patience How does this process work? 10,000-foot level: Sandmeyer reaction: Using Hydrochloric acid, combine GABA and sodium Nitrite. Convert them into GBL Now, the GBL molecule is floating in the solution as a non-polar molecule. Using DCM (Dichloromethane, AKA Methelyne Chloride) extract the GBL molecule INTO the DCM solution. Distill the DCM @ ~40C Distill the GBL @ ~150C (under vacuum) or 200C at sea level. Convert GBL to GHB Done!.

(4) Reagents and quantities: As an example: using 1mol of all your main reagents: 1 Mol pure GABA 1 Mol pure Sodium Nitrite NaNO2 (NOT Nitrate) 1.1 Mol concentrated Hydrochloric acid HCL(aq) 1250ml of DCM (Dichloromethane) (~ 6 * 210ml) ~233ml distilled water Some baking soda NaHCO3 (quantity to be determined based upon quantity of actual GBL extracted) Ok. So, lets calculate the actual grams and ml s required: 1 mol GABA = ~103.1g 1 mol Sodium Nitrite = ~69g 1.1 mol concentrated HCL (aq) (note: concentrated simply refers to 30-36% HCL at room temperature) = ~111.6ml (31%) 92.6ml (36%) NOTE: 31% HCL is roughly 9.6mols / liter and 36% HCL is roughly 12 mols / liter. Always try to use concentrated acid as this form of HCL has the least amount of water possible. You can get an idea of the molar quantity by looking on the bottle and finding the F.W (formula weight). 36.6 is 12 mol/L for instance. FW information can be found on the web. Many of the bottles are labeled differently. NOTE: Calculating the number of MOLES/LITER for HCL(aq): 1) Take the percentage and calculate the milliliters of a liter that the percentage represents: so, if you have 37% HCL(aq) that would equal 370ml in a liter solution. 2) Take that number: 370ml and multiply that times the average molecular density at room temperature (and sealevel): 1.12 = 414.4g 3) Take the average grams and divide it by the molecular weight of the acid: 36.46g/Mol: So, 414.4 / 36.46 = 11.4 moles roughly. NOTE: An important chemistry reminder, the number of significant digits for ANY calculation is only as good as the number with the lowest number of significant digits. So, in the preceding example, make sure you use: 370.00ml, 1.12 average density, and 36.46 g/mol for all your calculations. Sounds stupid, but is someone specifically gives you a number say: 12.1, they are implying that the maximum number of significant digits you can use is 1. So if you took the above example again and rounded up all the numbers: 370.0ml, 1.1 ad, and 36.5 g/ml your calculation would yield: 11.2 moles. From an accuracy standpoint, the calculation yields a big difference. Also, notice that textbooks refer to concentrated HCL as 12 molar solution. In reality it could be an 11 molar solution. That would affect the amount of acid you add to a mixture. In our.

(5) case, you would end up adding too little. With this reaction, always better to add too much.. A few notes on reagents: There are roughly 4 grades of reagents: Industrial (low grade, probably contains heavy metals) Technical (high grade) ACS (Very high grade, or at the very least analyzed and the heavy metal content is printed on the label) Food quality (Nothing harmful, but may contain fillers) Always go for technical or ACS if possible. At the very least make sure whatever you are buying has been analyzed for purity. For instance, you can buy GABA on EBAY in Ziploc bags for dirt-cheap. This stuff might be pretty good, as it s been purchased in bulk from a very high-grade manufacturer. ANY reagents with fillers WILL upset the reaction and may, in fact, completely ruin your yield. Do not buy from GNC. They have a bad reputation for selling food grade reagents with lots of fillers..

(6) Suggested equipment The following are only suggestions. I purchased high quality equipment simply because I was such a novice, I needed to have as few mistakes as possible. If you are an expert chemist, you can probably do this with a paper bag and a ball of twine. Glassware. Only buy glassware with 24/40 glass joints. Glass joints make it really easy to assemble the apparatus and ensure a good seal. 24/40 is a popular size. NOTE: Regarding 24/40 ground glass joints. They are a very precise fit. That means, if something like a sodium-based chemical is vaporized into the joint during a distillation operation, the joints could freeze together if you let the apparatus cool before dissembling. Getting these joints unfrozen is difficult. 1 X 1L flask 1 X 2L flask 1 X Distillation head 1 X double-jacketed distillation/Reflux condenser NOTE: I use a double-jacketed reflux condenser AS a distillation condenser. So, one piece of equipment performs double duty o 1 X 500ml separation funnel o Set of 4 graduated columns (10ml, 50ml, 100ml, 500ml or equivalent) o 1 X Vacuum adapter o o o o. Miscellaneous Magnetic stirring rods (Heavy) 1 X rubber cork 2 X 10 ¼ inner diameter rubber hosing Turkey baster Set of plastic funnels Buchner funnel (for vacuum distillation) Long glass thermometer 0-400C Clamps and stands Keck clamps (to hold the different glass pieces together) Aluminum foil Automobile AC insulation hosing Lots of paper towels Lots of rubber gloves Eye protection (industrial, not eye glasses) Spill absorbent material Non-powder chemical spill fire extinguisher (I have an old Halon unit, pre-ban) o Cleaning brushes o o o o o o o o o o o o o o o o.

(7) Mechanical stuff o Vacuum pump capable of ~23 inHg vacuum (23 inches of mercury is VERY easy to obtain. Even a crappy diaphragm pump can do this if it s in decent working order) o Manual vacuum pump. The kind purchased at a auto parts store with inHg scale. o Electric hotplate/ magnetic stirring device o Cheap 3-beam balance. This is not rocket science. Something that can measure roughly a tenth of a gram is sufficient. o PH meter or strips. I purchased a Exetech electronic PH meter. Just easier to use and very accurate. Good water supply (see picture below). I rigged up a PUR water purifier to be my distillation/reflux supply. Basically, I took the plastic adapter off a tube of glue and glued it to the PUR unit using Gorilla Glue (Gorilla glue can actually glue plastics, ceramic, and glass impressive stuff).

(8) Electronic PH meter. Turkey baster with rubber hose attached. Used for DCM extraction. NOTE: Immerse the rubber hose on the end of the baster in DCM for an hour prior to using it to extract. Then thoroughly rinse it. Some of the rubber and coloring will become dislodged due to DCM exposure. I learned this the hard way..

(9) Buchner funnel, vacuum flask and auto-vacuum pump with in Hg dial. El-cheapo 3-beam scale from EBAY works GREAT..

(10) Various bottlebrushes I use. Variac I use to control the ventilation motor.

(11) Grizzly industrial suction pump (normally used for sucking up wood dust). I use it for my main ventilation pump. NOTE: A heated magnetic stirring device is one of the wisest investments you can make. Being able to peg a temperature and keep a solution mixing under a variety of circumstances is incredibly useful. The unit I purchased is pretty expensive, but it has the added advantage of being able to heat the solution to a desired range and peg it there with no intervention. NOTE: Regarding the ventilation system. DCM vapors have a funny way of eating through just about any paints or plastics. It s a good idea to periodically check your vent motor impeller and all your hosing on a periodic basis and replace as necessary..

(12) Step 1: Sandmeyer Reaction The Sandmeyer reaction (RXN) is the process of slowly dripping a nitric acid into a solution with the intent of creating diazonium salts from amines. What this means to you is: You will be handling dangerous concentrations of HCL and potentially generating a very nasty gas called Nitrous Dioxide. NO2 naturally forms during the RXN when you allow the exothermic reaction to spiral out of control. In other words, while dripping acid into the solution, heat is generated. If that heat increases too much, a brown gas will form. When too much brown gas forms, you are exposing yourself to a VERY reactive, poisonous gas. NOTE: Important note about this reaction. Up to the 2 molar reagent masses, you will have a relatively easy time controlling NO2 gasses by stirring at a very rapid rate with a heavy stirring rod (rapid being 300rpm or greater). But, when the volume of the solution becomes rather large, the stirring rod will become unstable and start to fling itself all over the flask. This means you will need to slow down the stirring speed and the brown gas will evolve VERY rapidly. Beware. Additionally, the concentrations of HCL you will be handling will also generate a caustic gas at room temperature. SO! During this stage remember the following: Wear latex gloves and eyewear AND something that covers your arms before, during, and after the handling of concentrated HCL. This means wearing protection WHILE you are washing your glassware. Splashing concentrated HCL on you is not pleasant. Vent the area with STRONG ventilation. I purchased a high power shop vacuum from Grizzley industrial to handle the ventilation. Not the kind with a 3 in hose, but a 5 in hose. Industrial duty (meaning can run 24 hours a day). Your bathroom fan is not strong enough. Also, I control my vent with a variac transformer so I can vary the suction strength. Buy a organic vapor gas mask from Home depot (or equivalent). Professional painters use them. This mask may come in handy if something goes wrong and you need to shut off the dripping apparatus. Keep a chemical absorbent handy in a bag. If the apparatus tips over or leaks, you will have a real nasty chemical spill on your hands. Chemical absorbent will save you a lot of trouble. Since acid will be your main problem. Be prepared to apply A LOT of water to the spill and keep mopping. PH strips are handy here to test your floor for residual acid.. 1.1 Prepare your solution.

(13) Take your 1L flask and put it in a large Tupper wear container (PLASTIC! Glass dispels heat too fast, you will see why shortly). Put the flask and container on the magnetic stirring plate and fill the flask with the distilled water. Drop in a magnetic stirrer and set the stirring at 300 RPM Measure the GABA powder and add to the flask with a funnel. You may need to poke it through with a glass rod. Make sure the GABA is completely dissolved before continuing. Measure the Sodium Nitrite and add to the flask with a funnel. Same as with GABA. Take the flask off the stirring plate and observe the liquid. Swirl the flask until all the reagents have dissolved. If you still see crystal powder floating on the bottom of the flash, add 25ml of distilled water and swill again. Repeat until the solution looks like a clear yellowish liquid. Pack the Tupper wear with ice and enough water to reach the level of the solution inside the flask. Place a thermometer in the flask and allow the solution to chill until it reaches its minimum temperature (thermometer stops moving). For me, this appears to be about 5C.. 1.2 prepare your acid Chill the HCL in a refrigerator. A refrigerator that you don t store your food in (my god, if you store reagents with your food, please stop immediately and go watch an episode of Friends instead :P).. 1.3 Assemble your dripping apparatus Assemble the entire dripping apparatus first. Below is the apparatus I used. NOTE: I m using a separation flask because it has a PTFE valve. This allows for greater dripping control. The Chromic method suggests using a pressure equalized addition funnel. This is nice if you can find one with a PTFE valve. The reflux condenser is used to generate a cool air column, which cools and condenses the air immediately above the solution liquid line. Additionally, the cool downdraft created by the condenser displaces the NO2 gas and forces it up to the top where the vent can grab it. Additionally, I am placing a small notch on the PTFE valve hole using a sharp xacto knife. This notch helps fine tune the dripping rate. NOTE: Concentrated HCL will vaporize the second you open the bottle, EVEN if it s been previously refrigerated. THIS VAPOR IS GASSEOUS ACID. If you inhale it, you are in for a hell of a ride..

(14) Make sure the water supply to the reflux condenser is on and allow it to run for about 30 minutes to completely chill the air column You should be getting a general picture right about now: EVERYTHING needs to be very cool.. NOTE: The brownish color in the flask is NO2 gas. I made the mistake of not allowing the mixture and the acid to chill before beginning the process. Also, what you ca n t se e is t h a t t h e t op of t h e r e flu x colu m n is r igh t be low t h e m a in ve n t ..

(15) Make sure the dripping apparatus (PTFE valve in this case) is turned OFF . Pour the measured HCL into the dripping apparatus. Set the RPM on the stirring device to about 300-400 RPM. I have observed that evolution of brown gas is greatly reduced when the stirring is aggressive. But, if the amount of liquid is too great and the stirring rod is too small, your max RPM will be about 200rpm which is not nearly fast enough.. 1.4 Begin dripping Now, turn the valve VERY slowly and observe the bottom stem of the dripping apparatus. When a liquid start to drip, begin counting the seconds between drips. At the beginning of this procedure, you should have about 10 seconds between drips. After the first hour, decrease that to every 5 seconds, after the next hour, 3 seconds. Keep replacing the ice as it melts. It will melt fast as the solution is generating heat (exothermic). NOTE: During the dripping procedure, you need to pay very close attention to the apparatus, ESPECIALLY if you are using a glass stopcock addition funnel. If the glass stopcock is not properly clipped into the funnel, it could jar loose when the glass around it changes temperature. That could result in a disaster and the HCL could begin pouring into the solution. Yet another reason to use PTFE if you are an amateur. If you make a mistake and you accidentally allow a stream to enter the flask, shut off the valve, back out of the room and allow the gas to be vented. The reason for the initial slow drip rate is to retard the evolution of the NO2 gas. You WILL generate gas. But you can control it so the evolution will be very slow. After about one third of the acid has been added, the evolution will slow drastically, after the next third, even slower, etc. Just remember, the gas is evolving because of the temperature of the solution. Chilling, and mixing both assist in maintaining an even temp throughout the entire solution. When all the HCL has been dripped into the solution, replace the ice one final time and walk away from the experiment for 36 hours. The actual reaction occurs over time and needs as much time as possible. If you see tiny bubbles (nitrogen), the reaction is still taking place. You can stop it after 36 hours (continue onto the next step), or let it continue for another 12. The longer you let it sit, the more product you will be able to extract in the end..

(16) Step 2: DCM extraction NOTE: Chromic s method separates the water first to increase the yield. We are not going to do that in order to decrease the complexity of the method. If you follow these instructions, your yield will not noticeably go down and should stay at ~70%. Extracting with DCM. Clean your separation funnel first and get your 2L flask ready. You are going to break the DCM into 6 equal parts of 220ml each. The easy way to do this is to use a measuring column each time you need 220ml and simply keep track of the number of times you do the extraction (6). [BEGIN MAIN DCM EXTRACTION LOOP] Using a funnel pour 220ml of DCM into the main solution. Placing a rubber cork into the flask, carefully turn upside down (while holding the cork in place). Then, turn right side up. Pull the cork out and allow to vent (some DCM will vent). Shake/swirl the flask carefully allowing the solution and the DCM to commingle. When I say carefully, I mean, you have a heavy stirring rod in the solution. Breaking your flask with your stirring rod is really dumb. Do this shaking/swirling for about 60 seconds. Place the flask back on the stirring plate and set to 200RPM. Let this run for 30 mins. Using the turkey baster (or some similar suction device not your mouth ), tilt the flask on its side and suck out the DCM. Then, place the DCM into the separation funnel (make sure the valve is closed). The bottom layer in the funnel will be the heavy DCM. Open the valve carefully and allow that layer to flow into the 2L flask. There may be an intermediate layer that looks a little dirty or foamy. Leave that layer. Here is a picture of the funnel with the various layers. DCM on the bottom:.

(17) Pour the dirty layer and the top layer back into the 1L flask. Repeat until you get the majority of the DCM out. Go back to the main DCM extraction loop and repeat until you have repeated it 6 times. And you now have a 2L flask with lot s of DCM in it. Not necessarily.

(18) 1320ml Frankly, I m not sure how much DCM is lost or is still in the original solution. Save the original solution in a mason jar or some container. You may have screwed up and will need to repeat the procedure. You never know..

(19) Step 3: DCM Distillation Setup the apparatus as shown:. NOTE: I m using an extra piece of glassware called a fractionating column. Disregard this, as it s not necessary. Also, instead of the auto-AC-hose insulator, you can use aluminum foil. Additionally, you can see my 1L boiling flask used to capture the DCM. Forget this and use your regular 1L flat bottom flask..

(20) When assembling the apparatus, keep in mind you will need to remove the 1L flask in order to dump the contents back into the DCM containers. This will have to be done at least once during the distillation. Using Keck clamps makes it easy to pop off the flask, empty it and replace it. Also, the support stands are important as the entire glass assemble is heavy and will break if you allow it to all be supported by the main 2L flask. NOTE: The purpose of the insulator on the main distillation heads is to keep the DCM in a gas form until it hits the condenser. Once there, it converts back into a liquid. Without these insulators, you will have a lot of DCM dripping back into the main 2L flask. This is inefficient. Now that you have the apparatus assembled, turn on the water supply to the condenser and begin heating the hot plate. The distillation process will peg at a static temperature while it s vaporizing the lower temp solution (in this case DCM). DCM s initial boiling point is around 40-44C (measured in solution). It will be lower if you measure the actual vapor at the distillation head. So, be careful when turning on your hot plate. Especially if you don t have a thermometer as you might be like me (impatient) you will turn up the temperature very high until the DCM boils, but forget to turn down the temp afterwards. If the temperature is too high, you will eventually boil off the DCM and begin boiling the GBL. You don t want that yet. NOTE: Then most of the DCM has been vaporized; the remaining DCM can be vaporized by steadily increasing the solution temperature until no more solvent will come out of the solution (probably around 55C liquid temp). There will be some DCM left in solution, but that will evaporate during the next step. NOTE: A few thoughts about DCM. Saying DCM is a solvent is like saying plutonium is radioactive. This stuff will melt many plastics on contact in the liquid form. In a heated vapor form, you can suck the chrome off a Harley. I accidentally spilled about a ¼ cup on the counter top and my plastic stopwatch happened to be laying down there. I immediately dropped towels on the counter and picked up my stopwatch, it was melted...within seconds of exposure. Wearing latex gloves, I spilled a few tablespoons on my fingers, and within seconds my fingers began to burn. I pulled off the gloves and the DCM had magically passed right through the latex. BEWARE! This stuff is suspected of being carcinogenic. I wear an organic respirator when I handle it..

(21) Step 4: GBL Distillation FINALLY! Almost near the end. After distilling the DCM, you are left with a yellowish-orange liquid. IN theory, you should have over 100ml of solution at this point. The amount will vary with your patience during the DCM extraction phase. Setup the next apparatus. Guess what? It s the same setup as step 3. Leave the previous apparatus intact with the solution still in the 2L flask. Empty any remaining DCM into its original container (seal them all tight, DCM likes to escape). Clean the 1L flask.. Vacuum distillation The idea it this: Since GBL requires a high boiling temp (~200C sea level), you can lower the boiling temp by ~25C every time you halve the pressure inside the apparatus. So, at ½ the atmospheric pressure, the BP is about 175. ¼ it s about 150, 1/8 its about 125, and so on. Believe me when I say that the lower the boiling point, the better off you will be. Burned GBL is pretty horrific tasting, even if you reflux it with carbon. The following chart shows the measurements in TORR and inches of mercury (in Hg) Pressure 1/2 1/4 1/8 1/16 1/32. Torr @ Atmos. 760 760 760 760 760. Factor 2 4 8 16 32. Torr @ Factor 380 190 95 47.5 23.75. inHg at Torr 14.96 22.44 26.18 28.05 28.98. Degree Drop 25 50 75 100 125. So, if you wanted to bump down the BP to ~150C you would bring the vacuum down to 190 torr or 22.44 in Hg. By the way, a handy way to measure vacuum is to go down to an autoparts store and buy a vacuum pump with an inHg gague. I would not recommend manually operating the vacuum (using a hand pump) during the GBL distillation phase, a cheap electric pump will maintain a constant vacuum. That is crucial to a consistent and efficient recovery. The WHOLE reason for using a vacuum is to minimize the chance of burning the GBL. If GBL breaks down past 200C, then by distilling it at 150C you have a significant margin of error. In reality, get the vacuum as low as possible and this will increase the efficiency of the whole process by minimizing thermal loss. Which reminds me, it s really important to make sure you have plenty of aluminum foil surrounding everything even the top half of the flask. It s important to evaporate the GBL quickly and efficiently..

(22) Additionally, during the distillation process of GBL, the garbage left behind will most likely turn a dark brownish color. Don t worry, you are burning the sludge left behind and will not affect the quality of the distillate. NOTE: At this stage, it is very important to thoroughly insulate your flask and all the associated connecting glassware with aluminum foil (2 layers). This will accelerate the distillation process by keeping GBL in a vapor all the way to the condenser. Before placing the receiver flask on the apparatus, turn up the hot plate to about 150C and let the solution warm while stirring. Let it run like this for about 30mins. This will evaporate and vent the remaining DCM. Drop about 5-19 small absorbent charcoal pieces in the solution. This will force the solution to come to a roiling boil. Attach the receiver flask and turn on the vacuum pump. Begin slowly increasing the heat until the mixture starts to vigorously boil. Personally, I would allow the solution to boil until there is a thin layer of liquid left. I would not allow it to all evaporate leaving a hard crust on the flask. You would have a difficult time cleaning that. CAUTION!: When the GBL has been distilled, if you immediately disconnect the glasswork, be careful not to inhale the vaporized GBL. It will seriously burn your mucus membranes especially your sinuses. Congratulations! What you have at this point is semi-pure GBL. It still has impurities, including an acid that smells bad. But, in theory, you can ingest 1-3ml of the product and enjoy it as it stands. But, if you re not satisfied and want to do the right thing you need to take the final step and convert the GBL to GHB. There are several reasons to do this. The primary one is to increase your yield. A portion of GBL is ruined when it passes through your liver on the way to the kidneys. This is a waste and also stresses out your liver for no good reason. When you convert the GBL molecule to GHB, you increase its weight and you decrease the loss by way of the liver. You, in effect, increase your yield.. Step 5: GBL to GHB conversion (simple method) There are two methods to convert GBL to GHB: 1) Use NaOH (sodium hydroxide) 2) Use Baking soda (NaHCO3 ) Method 2 is the easiest. By easy I mean there are no caustic solutions and you have a lot of room for error..

(23) 5.1 Calculate the amount of baking soda and water required Now is the time to calculate the amount of Baking Soda required. The amount is equimolar. That is, you need an even amount of GBL and Baking soda by molecular weight (NOT weight in grams). So, the first step is to calculate the number of moles you have of GBL: Find the FW (formula weight) of your GBL solution NOTE: When converting volume to weight (ml to gram). You simply multiply the homogenous liquid by multiplying the milliliters * average density. The average density of GBL is 1.124 g/ml. So, lets say you have 100ml of solution, 100ml * 1.124g/ml = 112.4g It s that easy to convert from milliliters to grams! Use the web to find average densities of any molecule you are using. Now that you have the weight in grams, convert to moles by dividing the average weight in grams/mol which is 86.06g/mol. This info is also all over the web. So, 112.4g / 86.06 g/mol = ~ 1.3 moles Using your GBL FW, find the amount of Baking Soda required Now you know that your 100ml of solution weighs about 112.4 grams and contains about 1.3 moles of the GBL molecule. Now you need 1.3 moles of baking soda. Its average weight in g/mol is: 84.01 So, 1.3 * 84.01 = ~109.2g Find the rough amount of distilled water necessary Molecular weight of water is 18.015g/mol (round to one significant digit 18.0) Average density of water at 20C is about 1.0 19.8 moles H2O / 1 mole of Baking soda. 1.3 * 19.8 = 25.7 moles of water 25.7 * 18.0 = 463.7ml of water Total GBL = 100ml Baking Soda = 109.2 grams.

(24) Distilled water = 463.7 ml (500ml is fine) Theoretical GHB end-product In theory, this reaction is equimolar. Therefore; the following equation will give you the theoretical yield of GHB. GHB has a molecular weight of 126.1g/mol. Using the above example of 1.3 moles of GBL, do the following calculation: 1.3 * 126.1 = ~163.9g. 5.2 Prep the Baking Soda, water solution In a 1L Flask: Heat the water to a boil. Pour in the Baking Soda. Mix until all the baking soda is dissolved. The water will clarify when all the baking soda is dissolved. Reduce to a low boil. Pour in the GBL. The water will take on a light yellowish color.. 5.3 Reflux Place the reflux condenser on the flask and boil for about 30-60 minutes. Get the reflux condenser on the flask as soon as you place the GBL in the boiling solution you are loosing precious GBL every second you leave the system open to the atmosphere.. 5.4 Adjust PH After the 30-60 minutes of the reflux is up, test the PH. In general, you want it around 68. After the clarification stage, re-measure the PH again to be sure it s where you want. IDEALLY a PH of 7.5 will be the smoothest possible solution to ingest. PH adjustment: If the PH is to high: 9 lets say, add a small amount of GBL and reflux for 10 minutes. OR, you can add white distilled vinegar until the PH drops to about 8. For the most part, the clarification process will absorb the Vinegar smell. If the PH is too low, adding a little more Baking soda and refluxing should bring it up.. 5.5 Clarify.

(25) The refluxed product will most likely smell funny. This is due to residual butyric acid. Boiling the solution in charcoal will take care of any smells (plus any residual smells from the entire operation). Remove the reflux condenser and add 5% charcoal by volume. For example, if you have ~700ml of liquid, add 35ml of charcoal. Heat to a light boil for about 10 minutes. Pour the entire contents of the solution through a vacuum filtering apparatus (ATTACH PICTURE) When the solution if filtered, leave the charcoal in the filter and add about 3 X 50ml of distilled water to wash the charcoal of any GHB that has cooled on the surface of the charcoal.. 5.6 (Optional) Distill water and crystallize Place the flask with the solution on the hot plate and distill the water until the solution temperature is pushing about 150C. You will notice a drastic slow down in steam venting at this point (this is where the automatic hot plate comes in handy if you peg the temp at 150C, it will automatically cool down to maintain the temperature.) Layout a flat sheet of aluminum foil and curl up the edges on all four sides. Pour the solution onto the foil and allow solution to cool and crystallize..

(26) Quick calculations for various reagent quantities NOTE: Black numbers are for calculation purposes. Red numbers are actual quantities required. All numbers are rounded to a single decimal place. In chemistry, it s a good idea to keep decimal precision at the lowest common denominator when using multi-part equations. Because I don t know the truth, any number with nothing after the decimal point is assumed to have a .0 after it. NOTE: When experimenting with the 3mol reaction, I tried to lower the amount of DCM I was using by limiting the quantity to 6 times 500ml vs 6 times 600ml. Instead of 160ml theoretical yield, I got a 150ml yield. Something to consider Reagents required Reagent moles 0.5 1 1.5 2 2.5 3 FW of GABA (g/mol) 103.1 103.1 103.1 103.1 103.1 103.1 GABA (g) 51.6 103.1 154.7 206.2 257.8 309.3 FW of Sodium Nitrite (g/mol) 69 69 69 69 69 69 Sodium Nitrite (g) 34.5 69 103.5 138 172.5 207 Hydrochloric acid required (additional 0.1 mol / mol of reagent) 36% Hydrochloric Acid (ml) 45.8 91.7 137.5 183.3 229.2 275.0 31% Hydrochloric Acid (ml) 57.3 114.6 171.9 229.2 286.5 343.8 Water required to dissolve reagents Minimum water required (ml) 117 233 350 466 583 699 DCM required to extract the GBL Total DCM required 630 1260 1890 2520 3150 3780 Amount of DCM / extraction 105 210 315 420 525 630 Calculations for GABA to GBL reaction Percent yield estimate 0.7 0.7 0.7 0.7 0.7 0.7 FW of GBL (g/mol) 86.1 86.1 86.1 86.1 86.1 86.1 Average density of GBL (g/ml) 1.1 1.1 1.1 1.1 1.1 1.1 Possible GBL yield (g) 30.1 60.2 90.4 120.5 150.6 180.7 Possible GBL yield (ml) 26.8 53.6 80.4 107.2 134.0 160.8 Possible yield of GBL in Moles 0.4 0.7 1.1 1.4 1.8 2.1 Calculations for GBL to GHB conversion FW of Baking Soda (g/mol) 84 84 84 84 84 84 Baking soda required (g) 29.4 58.8 88.2 117.6 147.0 176.4 FW weight of water (g/mol) 18 18 18 18 18 18 Water factor / mol of baking soda 19.8 19.8 19.8 19.8 19.8 19.8 Minimum water required (ml) 124.7 249.5 374.2 499.0 623.7 748.4 Clarifying charcoal by volume (ml) 9.0 18.1 27.1 36.2 45.2 54.3 Final GHB yield FW of GHB (g/mol) 126.1 126.1 126.1 126.1 126.1 126.1 Possible GHB yield (g) 44.1 88.3 132.4 176.5 220.7 264.8. 3.5 4 103.1 103.1 360.9 412.4 69 69 241.5 276 320.8 366.7 401.0 458.3 1223 1864 4410 5040 735 840 0.7 0.7 86.1 86.1 1.1 1.1 210.8 241.0 187.6 214.4 2.5 2.8 85 208.3 18 19.8 873.2 63.5. 86 240.8 18 19.8 997.9 72.7. 127.1 128.1 311.4 358.7.

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