Gammabutyrolactone (GBL)

[nbk2000]

The reaction between tetrahydrofuran with trichloroisocyanuric acid at 0 °C, with the addition of water, produces gamma-butyrolactone (GBL).
Benicasa, M.; Grandi, R.; Ghelfi, F.; Pagnoni, U. M. Synth. Commun. 1995, 25, 3463.

For those who don't know what GBL is, that's an immediate precursor for GHB, better known as 'The Date-Rape Drug'. :o

Has the advantages, when properly prepared, of being tasteless, quick acting (less than 15 minutes), water and alcohol soluble, quickly eliminated from the body, and leaves the victim with amnesia of events having taken place immediately before and during the intoxication.

You can also use neat GBL for the same purpose, as this is the metabolic product of GHB breakdown, and the active ingredient, though it's a liquid and has a funky taste (so I've heard)

Fuck 'em silly, rob 'em blind, or snatch 'em up...all are doable and have been done with this type of drug.

What could be better than than to make a powerful knock-out drug from pool chlorinator and PVC pipe solvent? :)

Now all that's needed is someone to look up the requisite reference and do a little home lab experiment. ;)

BTW, while looking for this, I found a google cached page from the Rhodium archive where he (Rhodium) mentioned doing the same thing using HTH instead of TCAA (perhaps he confused the two?) and, naturally, some dumbass says "Why bother when you can buy GBL?".

Well, dumbass, you could buy GBL in '98 (date of the post), but you can't do that no mo'! So THAT'S why you learn how to make everything from anything, because the day WILL come when you can't buy nothing for anything. :p

And while we're at it, how about converting starting-fluid ether to ethyl acetate?
Juenge, E. C.; Beal, D. A. Tetrahedron Lett-. 1968, 55, 5819.

[Mumble]

Rhodium may not have been refering to the HTH shock product. HTH also makes a chlorination compound. And what ingredient does said chlorination compound contain you ask? Why Trichloroisocyanuric Acid of course.

I've seen this proceedure before. You could easily buy both precursors at wal-mart, no questions asked. They are trained to look for bulk ephedrine purchases, and people with gallons and gallons of acetone. They'll never see a container of PVC cement and a canister of organic pool chlorination as a warning sign. I mean I have bought the two there several times.

[megalomania]

I remember reading about a reaction to convert THF to GBL, but IIRC it was rather complex and not likely to be OTC. I may have been reading a different procedure than this, however. I just ordered supplies yesterday for the synthesis of 1,4-butanediol, the precursor of both THF and GBL.

[Dave Angel]

I have here a pdf of a paper on solvent free permanganate oxidations, which describes the use of combinations of KMnO4, CuSO4 and Alumina to oxidise among other things:

1,4-butanediol to gamma butyrolactone in a 95% yield over 14 hours.

Tetrahydrofuran to GBL in a 70% yield over 6 hours.

The components of the oxidant should be readily available to most; in the uk, alumina from ceramics supply and KMnO4/CuSO4 from the right garden centres - though I would be concerned about the purity of the end product with garden centre chems...

OT: There also seems to be potential for the ever elusive simple oxidation of primary alcohols to aldehydes - they manage pentanol to pentanal with 80% yield, perhaps there is hope for ethanol to acetaldehyde.

If the pdf attached is too big to be acceptable then the paper ref. is:

Tet. Lett. 42 (2001) 5833-5836

[tom haggen]

GHB is yet another chemical that has falling victim to the police state we are currently living in. I believe it is classified as a schedule 1 controlled substance, while I have read that it has great potential for the treatment of alcoholism. Coincidentally there is a thread over at MSDB going on about a synthesis of GBL from GABA and sodium nitrite. While the original post seemed quite shady, it would definitely be an easy route of obtaining GBL. While GHB is a date rape drug I believe the original date rape drug was rohypnol. I think its safe to say that GBL is a chemical that the government is going to have a hard time controlling.

[megalomania]

I have been interested in catalytic transfer hydrogenation as of late. There are some excellent articles in Rhodium's archive that describe using CTH with a microwave. I suppose it is worth a shot putting a beaker of purified 2-butene-1,4-diol, alcohol, and U-Ni-A (or B, I have not decided yet) in the microwave and see if it works.

I will have to take a closer look at the catalytic synthesis of formaldehyde as well. That is really the only important ingrediant in this synthesis.

If I have not detailed the reaction as of yet it is formaldehyde + acetylene + CuO (cat) --> 2-butene-1,4-diol
2-butene-1,4-diol + H2 + U-Ni-A (or U-Ni-B) (cat) --> 1,4-butanediol

If I had not dissolved my bubbler this reaction may have worked better for me. Now I have much more CuO to work with, and using nbk's teflon bubbler idea I will not fail.

BTW, I know the potassium permanganate used for water softners is quite pure (> 99%) since it involves human consumption as the intended use.

[Macgyver]

What other interesting things can GBL be used for besides drug manufacture?

(Happen to have some that I got a few years ago, while it was still available here in Europe).

[Macgyver]

What other interesting things can GBL be used for besides drug manufacture?

(Happen to have some that I got a few years ago, while it was still available here in Europe).

[Macgyver]

What other interesting things can GBL be used for besides drug manufacture?

(Happen to have some that I got a few years ago, while it was still available here in Europe).

[megalomania]

I believe its main use is as a solvent for electronic components. According to Ullmann's Encyclopedia: "Butyrolactone is important as an intermediate in the manufacture of pyrrolidone derivatives and as a solvent for polymers and agrochemicals."

[megalomania]

I believe its main use is as a solvent for electronic components. According to Ullmann's Encyclopedia: "Butyrolactone is important as an intermediate in the manufacture of pyrrolidone derivatives and as a solvent for polymers and agrochemicals."

[megalomania]

I believe its main use is as a solvent for electronic components. According to Ullmann's Encyclopedia: "Butyrolactone is important as an intermediate in the manufacture of pyrrolidone derivatives and as a solvent for polymers and agrochemicals."

[Macgyver]

I believe its main use is as a solvent for electronic components. According to Ullmann's Encyclopedia: "Butyrolactone is important as an intermediate in the manufacture of pyrrolidone derivatives and as a solvent for polymers and agrochemicals."

I got my GBL for cleaning circuitboards from flux ressidue after assembly, but I happened to order more than I needed, thats why I want to know if there's any other interesting uses if you're not into making drugs out of it.

(Probably have over 4 litres left). :D

[Macgyver]

I believe its main use is as a solvent for electronic components. According to Ullmann's Encyclopedia: "Butyrolactone is important as an intermediate in the manufacture of pyrrolidone derivatives and as a solvent for polymers and agrochemicals."

I got my GBL for cleaning circuitboards from flux ressidue after assembly, but I happened to order more than I needed, thats why I want to know if there's any other interesting uses if you're not into making drugs out of it.

(Probably have over 4 litres left). :D

[Macgyver]

I believe its main use is as a solvent for electronic components. According to Ullmann's Encyclopedia: "Butyrolactone is important as an intermediate in the manufacture of pyrrolidone derivatives and as a solvent for polymers and agrochemicals."

I got my GBL for cleaning circuitboards from flux ressidue after assembly, but I happened to order more than I needed, thats why I want to know if there's any other interesting uses if you're not into making drugs out of it.

(Probably have over 4 litres left). :D

[trinitride3]

NBK I was wondering if you could post the exact synthesis for GBL using tetrahydrofuran and trichloroisocyanuric acid. I haven't had any luck finding it over at rhodium. much appreciation

[trinitride3]

NBK I was wondering if you could post the exact synthesis for GBL using tetrahydrofuran and trichloroisocyanuric acid. I haven't had any luck finding it over at rhodium. much appreciation

[trinitride3]

NBK I was wondering if you could post the exact synthesis for GBL using tetrahydrofuran and trichloroisocyanuric acid. I haven't had any luck finding it over at rhodium. much appreciation

[FUTI]

corn cob...furfural...furan...THF....1,4-butandiol...GBL
loooong procedure but obtainable by almost everyone.

[FUTI]

corn cob...furfural...furan...THF....1,4-butandiol...GBL
loooong procedure but obtainable by almost everyone.

[FUTI]

corn cob...furfural...furan...THF....1,4-butandiol...GBL
loooong procedure but obtainable by almost everyone.

[trinitride3]

NBK, could you please tell me the specifics regarding the reaction. Im looking to find the correct proportions of tetrahydrofuran and trichloroisocyanuric acid I need to use and also time for the reaction to take place before the water is added. I've searched extensively for this information at Rhodium and all over the web but haven't had any luck locating it. I would greatly appreciate any info you might be able to provide.

[trinitride3]

NBK, could you please tell me the specifics regarding the reaction. Im looking to find the correct proportions of tetrahydrofuran and trichloroisocyanuric acid I need to use and also time for the reaction to take place before the water is added. I've searched extensively for this information at Rhodium and all over the web but haven't had any luck locating it. I would greatly appreciate any info you might be able to provide.

[trinitride3]

NBK, could you please tell me the specifics regarding the reaction. Im looking to find the correct proportions of tetrahydrofuran and trichloroisocyanuric acid I need to use and also time for the reaction to take place before the water is added. I've searched extensively for this information at Rhodium and all over the web but haven't had any luck locating it. I would greatly appreciate any info you might be able to provide.

[nbk2000]

If you're going to try it and report back the results, then I'll get you the specifics.

From memory, the THF and water are premixed, and .15 moles of TCCA per mole of THF are used, and stirred while cooled to about 3°C, and the TCCA added in small amounts over the course of hours, stirring for 24 hours while allowing to warm up to room temperature an hour after the last TCCA addition.

I'll find the specifics later.

[nbk2000]

If you're going to try it and report back the results, then I'll get you the specifics.

From memory, the THF and water are premixed, and .15 moles of TCCA per mole of THF are used, and stirred while cooled to about 3°C, and the TCCA added in small amounts over the course of hours, stirring for 24 hours while allowing to warm up to room temperature an hour after the last TCCA addition.

I'll find the specifics later.

[nbk2000]

If you're going to try it and report back the results, then I'll get you the specifics.

From memory, the THF and water are premixed, and .15 moles of TCCA per mole of THF are used, and stirred while cooled to about 3°C, and the TCCA added in small amounts over the course of hours, stirring for 24 hours while allowing to warm up to room temperature an hour after the last TCCA addition.

I'll find the specifics later.

[nbk2000]

In order to moderate the reaction, the reaction flask was placed in an ice bath. To 60 ml (53.28 g, 0.74 mole) of tetrahydrofuran, containing 6 ml of water, was added 23.24 g (0.10 mole) of trichloroisocyanuric acid at such a rate as to maintain a gentle reflux.

Upon addition of the first amount of trichloroisocyanuric acid, a yellow color appeared and quickly faded. A white precipitate formed immediately. After all of the trichloroisocyanuric acid was added, the reaction mixture was allowed to stir overnight. Cyanuric acid precipitated almost quantitatively and was removed by filtration.

The filtrate was combined with 60 ml of ether and extracted three times with 20-ml portions of 5% aqueous sodium bicarbonate. The ether layer was distilled, and found to contain only tetrahydrofuran.

The water layer was acidified with aqueous hydrochloric acid, and the water and hydrochloric acid were removed by azeotropic distillation with benzene.

The benzene was removed by distillation, leaving 2.55 g (19%) of gamma-butyrolactone, bp 88-89ºC (10 mm).

[nbk2000]

In order to moderate the reaction, the reaction flask was placed in an ice bath. To 60 ml (53.28 g, 0.74 mole) of tetrahydrofuran, containing 6 ml of water, was added 23.24 g (0.10 mole) of trichloroisocyanuric acid at such a rate as to maintain a gentle reflux.

Upon addition of the first amount of trichloroisocyanuric acid, a yellow color appeared and quickly faded. A white precipitate formed immediately. After all of the trichloroisocyanuric acid was added, the reaction mixture was allowed to stir overnight. Cyanuric acid precipitated almost quantitatively and was removed by filtration.

The filtrate was combined with 60 ml of ether and extracted three times with 20-ml portions of 5% aqueous sodium bicarbonate. The ether layer was distilled, and found to contain only tetrahydrofuran.

The water layer was acidified with aqueous hydrochloric acid, and the water and hydrochloric acid were removed by azeotropic distillation with benzene.

The benzene was removed by distillation, leaving 2.55 g (19%) of gamma-butyrolactone, bp 88-89ºC (10 mm).

[nbk2000]

In order to moderate the reaction, the reaction flask was placed in an ice bath. To 60 ml (53.28 g, 0.74 mole) of tetrahydrofuran, containing 6 ml of water, was added 23.24 g (0.10 mole) of trichloroisocyanuric acid at such a rate as to maintain a gentle reflux.

Upon addition of the first amount of trichloroisocyanuric acid, a yellow color appeared and quickly faded. A white precipitate formed immediately. After all of the trichloroisocyanuric acid was added, the reaction mixture was allowed to stir overnight. Cyanuric acid precipitated almost quantitatively and was removed by filtration.

The filtrate was combined with 60 ml of ether and extracted three times with 20-ml portions of 5% aqueous sodium bicarbonate. The ether layer was distilled, and found to contain only tetrahydrofuran.

The water layer was acidified with aqueous hydrochloric acid, and the water and hydrochloric acid were removed by azeotropic distillation with benzene.

The benzene was removed by distillation, leaving 2.55 g (19%) of gamma-butyrolactone, bp 88-89ºC (10 mm).

[MushroomMarkk]

I was unaware that THF could be picked up at walmart! Its a little off topic I believe, but could someone mention the brand name that THF is under. Unless I misunderstood something :( that would be a dissapointment.

+++++++++

This would be considered a spoonfeeding request and cause for banning. Don't repeat the mistake of asking for something that you can easily find out for yourself with a little bit of UTFSE.

[Hobbit Porn]

On a completely unrelated forum, one of the posters put up this link
http://www.alloycleaner.com/
I Had a read around the site, and they are based out of the UK.

IIRC (please someone correct me if this is incorrect), 1,4-butanediol is metabolised in the body to GHB. If this is correct, it would probably be just as easy to focus on procuring 1,4-butanediol rather then GBL, since 1,4-butanediol is a very commonly used industrial solvent (at least in Australia).

[nbk2000]

Here, the butanediol is regulated the same as the GBL, so if you can get either of the two, getting the straight GBL is to be preferred, as it's a much better product.

[nbk2000]

Finally a toxic chinese toy that's useful. :)

Better hurry though, they're getting pulled off the shelves.

Australian scientists say a chemical coating on the beads, when ingested, metabolizes into the so-called date-rape drug gamma hydroxy butyrate. When eaten, the compound - made from common and easily available ingredients - can induce unconsciousness, seizures, drowsiness, coma and death.

At least five children in the United States and Australia have been hospitalized after swallowing the toy beads, which are used in arts and crafts projects. They can be arranged into designs and fused when sprayed with water.

...

The toys are called Bindeez in Australia, where they were named toy of the year at an industry function this year, and in the United States they go by the name Aqua Dots.

http://www.newnation.vg/forums/showthread.php?p=223002#post223002

[bloodbob]

I wonder if you could get reasonable yields substituting the alumina matrix with silica or at least a zeolite.

[spetsnaz08]

http://www.mindandmuscle.net/forum/lofiversion/index.php/t8423.html

Dont break any laws, this is just for entertainment purposes:

GABA to GBL writeup
**this writup is only preliminary, and mainly is to facilitate perfection of this method **


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Introduction:

First of all, MANY MANY thanks to Chromic for helping to pioneer this method. This is simply without a doubt one of the easiest methods to make GBL for the clandestine chemist. Through some trial and much error, respectable yields finally have been obtained.


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Chemicals (in relation/ratio to the main precursor, GABA):

1 part Powdered GABA ( *** Do *NOT* use @NC brand GABA. Although many nutritional stores claim there are no adulterants, there most definitely are. )

0.68 part Sodium Nitrite (*** NOT NITRATE)

0.5 part conc H2SO4 (H2SO4 is sulfuric acid)

(in other words, GABA:Sodium Nitrite:H2SO4 1:0.68:0.5)

ACS NaOH or Baking Soda ( ** if you cannot get ACS NaOH, USE BAKING SODA

DCM (possibly other solvent, let us know if any others work!) (dcm is dichloromethane, methylene chloride, CH2Cl2, non-polar solvent)




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Procedure:

1. Dissolve GABA and Sodium Nitrite in a flash with water in an ice bath.

2. Make a mixture of 1 part conc H2SO4 2 parts water.

3. Put this mixture in a bottle capable of dripping VERY slowly (swif uses those red and yellow plastic ketchup and mustard bottles).

4. With stirring/swirling, let the H2SO4/water mixture drips very slowly into the GABA/NaNO2 mixture until all of it is used up. **IF YOU SEE BROWN GASSES, YOU ARE GOING TOO FAST -- THESE GASSES ARE POISONOUS **

5. Put the flask outside or somehow vent it outside as some of the gasses emitted are also poisonous and let sit for at least a day, 2 is preferable. You should see little bubbles of N2 being formed in the flask.

6. Now you need to convert all of the GHB/GBL into NaGHB so we can boil off all of the liquid. The GBL will steam distill, so that is why we convert it to NaGHB. You can add about 0.90 parts (compared to the original GABA) baking soda and reflux for 30 minutes to an hour. Alternatively, (swif's method of choice) you can use ACS NaOH (not lye) until the pH is neutral (7-8, a little more basic than neutral is OK).

7. Boil off about half of the solvent and add 1 part H2SO4. This is to destroy any dangerous nitrosamines and to convert the NaGHB back to GBL.

8. Extract the GBL with DCM ( uncertain if any other solvents will work, eg toulene, xylene) two or three times and combine the extracts.

9. Now you must separate the DCM from the GBL. One easy way of doing this is to prepare a boiling water bath and place the flask in there. The DCM will boil away, but the GBL will remain since its boiling point is much higher. *NOTE*

10. What you have left is GBL and some impurities. You can distill out the GBL at 200 deg. celcius. (Obviously, you cannot use the water bath ) *NOTE*

11. Congratulations! You have successfully made GBL. You can consume as-is, or convert to to Na/K GHB. An active dose is 1-2mL of GBL. GBL is a harsh mucous membrane irritant; be sure to dilute it in something! Enjoy!

*NOTE* There is another hypothetical method of separation that has not been tested yet. If it works, let us know! Titrate the DCM/GBL mixture with 50% NaOH and when the water is pH 8 or so, separate the water, and add enough vinegar until it is pH7 again.

Again, many thanks to Chromic and the hive in general for all the help in helping to formulate this procedure!






You can find the whole right up and some tweeks on the method at the hive . UTFSE and look under Success making GBL! . THere you should be able to put it all together and from the looks of it you can "dream" of making TONZ of gbl for really cheap. Of couse this is only in your dreams if you live in the military state called usa