gaba to gbl, an almost complete write up with pics

Soap · Thu Sep 01, 2005 9:11 pm

i helped some guy complete this synth way back when. i promised to do the write up but im a slacker... he did it all. since then i havnt seen him around and peeps have been asking for help on the synth so im gogin to post what he had done. as far as i know the purity of the gbl is still inquestion though i have tried it numerous times and was happy with the results. shit ill have to get the pictures in later, im low on time right now, there not that important anyway.

Modified GABA to GBL conversion and
extraction method for amateur chemists
By Cleaver, February 2005
Original chemistry and methodology by
Chromic
Introduction:
Welcome amateur chemists! I have performed the GABA to GBL conversion several
times using this method and it works very nicely. MANY thanks to Chromic for the
initial conversion process documentation.
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 Methylene 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!

Reagents and quantities:
1 Mol pure GABA
1 Mol pure Sodium Nitrite NaNO2 (NOT Nitrate)
1 Mol concentrated Hydrochloric acid HCL(aq)
1320ml of DCM (Dichloromethane)
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 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.
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.
o 1 X 1L flask
o 1 X 2L flask
o 1 X Distillation head (attach picture)
o 1 X Distillation/Reflux condenser (attach picture)
o 1 X 500ml separation funnel (attach picture)
o Set of 4 measuring columns (10ml, 50ml, 100ml, 500ml or equivalent)
o 1 X Vacuum adapter (attach picture)
Miscellaneous
o 1 X rubber cork
o 2 X 10 ¼ inner diameter rubber hosing
o Set of plastic funnels
o Long glass thermometer 0-400C
o Clamps and stands
o Keck clamps (to hold the different glass pieces together)
o Aluminum foil
o Automobile AC insulation hosing
o Lots of paper towels
o Lots of rubber gloves
o Eye protection (industrial, not eye glasses)
o Spill absorbent material
o Non-powder chemical spill fire extinguisher (I have an old Halon unit,
pre-ban)
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 Electric hotplate/ magnetic stirring device
o EBAY special 3-beam balance. This is not rocket science.
Good water supply. 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)

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.

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.
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 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.
Step 1.1 Prepare your solution
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.

When the whole solution looks like is has turned to 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 it s
minimum temperature (thermometer stops moving).
Step 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 Razz

).
Step 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.
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 can t see is that the
top of the reflux column is right below the main vent.
Make sure the dripping apparatus (PTFE valve in this case) is turned OFF .

Pour the measured HCL into the dripping apparatus.
Step 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).
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.

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. You will loose some
yield, but not much.
This is the weird part. 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:

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.

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.

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.

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.
The following chart shows the measurements in TORR and inches of mercury (in Hg)
Pressure Torr @ Atmos. Factor Torr @ Factor inHg at Torr
Degree Drop
1/2 760 2 380 14.96 25
1/4 760 4 190 22.44 50
1/8 760 8 95 26.18 75
1/16 760 16 47.5 28.05 100
1/32 760 32 23.75 28.98 125
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 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.
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.
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.
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:
GBL in milliliters * 1.124 gms/ml (average density at sea level)
So, lets say you have 100ml, 100 * 1.124 = 112.4g

Now that you have the weight in grams, convert to moles by dividing the average weight
in grams/mol which is 86.06g/mol
So, 112.4 / 86.06 = ~ 1.3 moles
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
1125ml water??
H2O molecular weight is 18.015, average density is about 1.00g/ml
1125 * 1 = 1125g. 1125/18.015 = ~64.4 moles
5.1) Calculate the amount of baking soda required
5.2) Reflux
5.3) Clarify
5.4) (Optional) Distill water and crystallize

beetle · Sat Sep 03, 2005 12:00 am

Thanks Soap, this is a beautiful story. SWIM will definitely look into this process and come back with some questions.

Gracias senior

icecool · Insistent Chemist

Maybe a stupid question but what is GABA?

Radiumhero · Sat Sep 03, 2005 12:27 am

Gamma-aminobutyric-acid

anime · Sat Sep 03, 2005 12:59 am

Its sold at health shops, its used for body building etc...etc.. ghb was also used for body building Smile

Soap · Sat Sep 03, 2005 11:19 pm

gaba can be found at almost all health food stores. the major nutirion center (hint) around here in the states offers a product that is very low quality. it claims that it contains nothing but gaba, but it has so much gak in it a synth with the stuff hardly ever works. swim bought 2kg of gaba through a common online auction for $25. tahts a good deal of gbl for taht price. swim has not looked into using sodium nitrite from meat supplies, so hes not sure if its pure enough to use.

icecool · Insistent Chemist

I might have seen this before IIRC I'm going to check on monday if it is GABA.
If so then I would bee very happy, since I can get NaNO2 very cheap HCl also very cheap and non-polar solvent too Smile

w00t....

Soap · Sun Sep 04, 2005 6:36 am

i have yet to meet another person that enjoys the effects of gaba. but personaly if i have to sit down to write an english paper, or anything else that requires some creativity, gaba is my favorite. i ramble to much when i smoke pot, gaba makes me focus. this is proably a subject for another thread but since where on the subject of gaba, does anyone enjoy it?

i cant stress enough the importance of cleaning this stuff, also the fumes it produces are nasty, so do the reaction somwhere were no one (not even the mean neighbors...) will be breathing this stuff. activated charcoal can be bought from the pet store next to all the fish stuff. its quality is in question though it is waht i have used with success.

methyl_ethyl · Riedel De Haen

Please everyone be careful with the final product of the synth. AFAIK, no one has had the time or resources to determine what that nasty sour "impurity", "contaminant" or "side reaction" is that is almost impossible to remove, and seems to be ever-present in the final product. I really would not suggest ingesting this substance. Yes the effects will be there, but who knows what else you could be doing to yourself, and god help you whoever you decide to give this stuff to, and god damn you if you actually try to sell this product to anyone as GHB.

What I have always feared most about this synth is that it appears to be a very easy synth for the amateur chemist, and even worse requires extremely easy to procure reagents. The product of this synth needs to be characterized before everyone decides they found an easy route to GHB.

So put your analytical hats on, synth this product, and characterize it, but please don't continue to ingest this shite until we all know what else is in the final product.

And please do not take any of Soap's warnings lightheartedly!!!!

regards,

m_e

stooge · Sun Sep 04, 2005 3:44 pm

Much more of a problem then getting GABA is obtaining Sodium Nitrite (NaNO2) for Swis ...

he found some info it can be obtained by mixing Nitrous Acid with NaCL, is this correct?
Are there some more infos to find on how to do this?

Thanks!

methyl_ethyl · Riedel De Haen

Good luck finding Nitrous Acid commercially, due to it's instability it must be prepared in situ, which is what the above procedure outlines.

Keep looking, Sodium Nitrite is very easy to source, check the hive files, there should be some easy routes to sodium nitrite, or hints on how to find a commercial source.

m_e

stooge · Sun Sep 04, 2005 10:19 pm

Thanks!

But finding a comercial source is hard in so far that it is not sold here to privat persons ...

will check the hive-files!

stooge · Thu Sep 15, 2005 2:02 am

pressumed that nitric acid (or is it nitrous acid??) is available - might be NH4NO3 (ger.:Kalkammonsalpeter) of any use in this task to produce sodium nitrite?
or elseway of any other use at all?

amenselah · Sun Sep 25, 2005 2:39 am

GABA ..high quality is very expensive ..I would recommend to experiment with cheap reagents....

Sodium Nitrite ..chek ebay..

loki · guinea pig

i don't understand what people are saying about nitrite being hard to find. along with sodium sulfite these are the two most common preservatives added to meat products. both chemicals are nasty and some people are sensitive to it (me being one of these) and i get very upset guts when i consume a lot of food laced with nitrite/sulfite. a key sign of a bad reaction to either of these chemicals is in the evolution of the respective gases that comes out when they decompose, sulfite forms sulfur dioxide and nitrite forms nitrogen dioxide, in the colon, and the subsequent venting of the gases produce eggy farts (sulfite) or stinking rotton ugh garbage bin smell (nitrite).