Sodium GHB
Procedure:
Dissolve 130 grams (3.25 moles) of pure sodium hydroxide in 400ml of tap water in a 1000ml glass container while stirring with a glass rod or similar. The dissolution is exothermic, and the solution will heat up. When everything has dissolved to form a clear solution, slowly add 250ml (280 g, 3.25 moles) of gamma-butyrolactone in 50 ml portions with good stirring. The addition of gamma-butyrolactone to the sodium hydroxide solution is also exothermic, and if it is added too fast the solution will begin to boil, and we don't want that. Keep track of the temperature with an immersed thermometer. The addition of the gamma-butyrolactone will take somewhere between 20-30 minutes. When everything has been added, let the mixture react for an additional 10 minutes with occasional stirring.
Now it is time to see if the reaction has gone to completion by checking the pH with universal pH paper. We are aiming for a pH of 7-8. If it is too high (pH > 8), then add 10 ml of gamma-butyrolactone and let react for a few minutes more. If the pH is too low (pH Na2CO3 + H2O + CO2
Reduce the heat to a light boil, and slowly add 250ml gamma-Butyrolactone (280g, 3.25 moles). The addition is not immediately exothermic as with the sodium hydroxide synthesis. Keep this solution at a light boil for 30 minutes. Check the pH with universal pH paper. We are aiming for a pH around 7, but anything 6 to 8 is perfectly safe. If the pH is too high, add a small amount more GBL and continue to reflux.
The solution will be perfectly clear and should be absolutely colorless. If it is not perfectly colorless, i.e. if slightly impure butyrolactone was used and the solution has taken on a light yellow color, add about 100 mL of activated charcoal. Allow this to boil for 10 minutes. Cool the solution then filter, washing the activated charcoal two or three times with 50 ml portions of cold water. 410g of NaGHB will be made in this synthesis. This solution can be concentrated to about 50% NaGHB before it will start to crystallize. If you wish for a powder, heat until the temperature of the solution reaches 150°C then pour onto a flexible metal sheet and allow it to cool and solidify.
This synthesis is perfect for use where there is no ACS, Food or Electronics grade sodium hydroxide available.
Literature methods
Sodium GHB has been made from NaOH and butyrolactone in water[8], in methanol[10,11], and aqueous ethanol[12]
Potassium GHB
Use the ethanol synthesis described above for sodium GHB, but substitute the 130 grams of NaOH for 182 grams of KOH (This calculation is based on the heavier K atom, and the higher water content of KOH versus NaOH). Using KOH gives users of K-GHB that Potassium supplement that is by some said to be needed in connection with administration of GHB. Bear in mind that (powdered) K-GHB is slightly less active (by weight) than Na-GHB as the K ion is heavier than the Na counterpart. Differences between K-GHB and Na-GHB is that the K salt is more soluble in water than the Na salt, and the taste is more like salt/licorice instead of the salt/soap taste of Na-GHB. In the book "Better Sex Through Chemistry" by J. Morgenthaler it is pointed out that "[GHB] has a salty/licorice flavor" and it is obvious that the author tried the K salt.
Calcium GHB [5]
74 g analytically pure calcium hydroxide are suspended in 200 ml of tap water. 160 ml 4-butyrolactone are added in portions (each portion about 5 to 10 ml) and under stirring to this suspension at room temperature. After addition of 20 ml the reaction mixture warms to about 50° to 60°C. The addition of 4-butyrolactone is controlled such that the temperature remains between about 50° and 60°C, which takes about 1 hour. During this time the calcium hydroxide has dissolved practically completely. The reaction material is contaminated with a slight rust-yellow precipitate. It is thinned down with 300 ml methanol, is left for four hours to itself and is then filtered through a folded filter. The clear filtrate is cautiously treated with 200 ml acetone in the way that after each portion of acetone causing a precipitate time is allowed for the precipitate to redissolve. A waterclear solution is obtained which is placed for crystallization. After two hours of standing colorless crystals start to deposit. In this state the crystallization is accelerated by continuous addition of acetone (in total 100 ml). The crystallization time is 24 hours. The crystals are sucked off and are washed initially with 50 ml methanol and then additionally with 60 ml acetone. The crystals are dried at temperatures from about 60° to 80°C. in a drying cabinet. Yield: 230 g. Melting point 166-168°C. (immediately). The product is the waterfree nonhygroscopic calcium salt of the 4-hydroxybutyric acid. It is dissolvable as desired in water, the aqueous solution has a pH- value of 7 to 7.5. The salt can be stored as long as desired and does not change in air. Even upon storage no water is attracted from the air.
The residue crystallizes to a mass of colorless crystals, which is after dried at temperatures from about 60° to 80°C. Yield: about 105 g. Melting point 164-166°C. The product is Di-(4-hydroxybutyric) calcium. It is recrystallized by dissolving in little methanol followed by adding of acetone to cloudiness, and crystallizing in the cold.
Instead of methanol also ethanol and isopropanol can be employed for recrystallization with the same success. Without employing water containing alcohols as recrystallization medium or as additive of the recrystallization and purification no stable and in particular no nonhygroscopic calcium salts are obtained. The water content of the alcohols should be from about 3-10% by volume. The such obtained final product does easily dissolve in water, is not hydroscopic and has a pleasant aromatic odor.
Magnesium GHB [5]
60 g magnesium hydroxide (analytical grade) are suspended in 200 ml tap water under stirring. In a stream and under stirring 160 ml butyrolactone are mixed into this suspension. Then the mixture is heated on a water bath for 6 hours under stirring in a 2-liter-flask. The magnesium hydroxide dissolves practically completely. The flask is allowed to stand overnight, while contaminants deposit and the solution is decanted without effort from the contaminant deposit. The water clear decantate is initially stirred with 100 ml acetone for 10 minutes. The colorless sirupy liquid, which now turned more viscous, is mixed again with 100 ml acetone as described above, the acetone is again removed by decanting and the fairly viscous, colorless sirup is left to itself at room temperature for about 2 to 4 hours. It solidifies to a colorless crystal mass, which is comminuted in a mortar and dried for several hours in air. Melting point 76°C to 78°C. Yield: 314 g in analytically pure form.
This magnesium salt contains about 5 mole of water of hydration. It is not hydroscopic, is stable and can be stored for arbitrary long times. By drying over several hours at 40° to 50°C it loses part of its water (1 mole) of crystallization and then melts at 118° to 120°C. Waterfree magnesium 4-hydroxybutyrate can be produced by removal of water by sublimation and/or evaporation of water under decreased partial pressure of water and at elevated temperature or by crystallization from a solution containing an organic solvent. The waterfree salt melts at 172-174°C. The chemical analysis shows 10.50 weight percent magnesium (calculated 10.55 weight percent magnesium). All modifications are nonhygroscopic and stable during storage. 1g of the magnesium salt dissolves in 2 ml water at room temperature, the pH of the aqueous solution is 7.
It dissolves easily in water, methanol and ethanol, it does not dissolve in ether and hydrocarbons, it is not hygroscopic, is storable and has a pleasant aromatic odor.
Other salts
The Lithium and Ammonium salts of GHB would be dangerous to ingest. Lithium ion is toxic, and together with NH3 lactone becomes pyrrolidone.
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