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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.
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
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!
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.
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 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
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)
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.
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.
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.
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 .
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.
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
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.
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.
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 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.
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 the atmospheric pressure, the BP is about 175. 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.
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.
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
5.3 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
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.
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