GHB from GBL & baking soda

[Chromic]

Just browsing the newsgroups, and came across:

http://groups.google.com/groups?hl=en&selm=20011228060021.10093.00000948%40mb-cm.aol.com

I thought that since the Hive isn't accepting new members, that I'd throw it up for discussion.

I remember asking a long time ago if this would work, but attempted only a short reaction time (30 mins or something), and it didn't work. It appears that sodium carbonate (the decomposition product of boiling sodium bicarbonate in water) is a strong enough base to react with GBL. Cool stuff, now no one has an excuse to use drain cleaner lye. (even though the reaction does take 36hrs of reflux)

Has anyone here at The Hive done something similiar to this?All of the recpies that use NaOH to make G have the same problem the reaction only goes about half way leaving lots of unreacted lactone in the mixture.

If you've ever had pure ghb or powder(pharm-grade) ghb you do notice a difference in effects and also have less side effects(headaches etc.), also there will be no smell at all in your ghb and the taste will be better if it doesn't contain lactone. There are a whole slew of reasons for wanting g without lactone and I could go on and on.. also when you use this method since the reaction goes to 100% na-ghb you get more mileage(products) out of your lactone...

Also not using caustic chemicals eliminates alot of headaches and even if you screw up the worst that would happen is a mixture of baking soda lactone and water which is not very bad compared with swallowing a posion (which people have done and been hospitalized for as seen in MM2K etc.) Also good about this recipe is that you know how much final grams of na-ghb you're going to have you will better be able to determine dosing....... When using an NaOH recipe results can vary due to the nature of the reaction and you end up with batches of various potency etc.

It is also easier to measure the ingredients,baking soda is of high purity and available for almost nothing at your local grocery store and you can easily make a powdered ghb simply by boiling the water away and letting dry...

Making NaGHB with baking soda and Lactone and water in a crock pot.... The only real problem with this recipe is that it takes time for it to happen, the reaction happens gradually thus allowing all the reactants to react if you give it enough time thus leaving you with no traces of lactone etc. the final product will smell like water and the taste will be nicer then your used to if your used to g made with NaOH...If all you have is lactone and you wanted some right away you could make some with NaOH, then use what you'd like then dump that mix into a crock pot add some baking soda and get the rest of the lactone to react and purify/clean your g mix up...(note: SWIM has yet to do that, though his plan might be to make some G with KOH and make some NAGHB with baking soda then add the K-GHB to crockpot add additional baking soda to react with lactone in the KGHB and have a k/Na g mixture without any lactone/impurities)..

The recipe is very simple..and a crock pot can be bought from walmart for $9.99...

1 part GBL
1 part Baking soda
2 parts water
(example: 250g GBL,250g arm+hammer,500mL H2O)

(trivia: sodium bicarbonate is 84g's per mole and butyrolactone is 86g's per mole, thus the above combination will give you a slight excess of baking soda thus making sure all the GBL reacts, if you put say only .9 parts Baking soda for 1 part GBL then you'd have some left over unreacted lactone.. not good! you
might want to put in a few extra grams baking soda just to be double sure...) dump ingredients together into the crock pot...turn the crockpot on low heat,

you must cover the crock pot with a bowl and then fill that bowl up with water, this will keep the lid cool and let the lactone drip back down into the solution so you don't waste lactone by boiling it off, if anyone wants a little picture or diagram of this let me know! It's really simple just put a big ceramic bowl from your cabinet on the top of the crockpot acting as your lid and pour water into the bowl..(the water will slowly boil away and you should add more to the bowl whenever you get a chance, if you come home and find the bowl empty NBD just fill it back up and everything should still be fine, perhaps a tiny bit or reactants/product may have escaped but probably not much and very possibly none at all)

You then leave this crockpot on LOW heat for 36 hours and all the reactants will go thru to final product...SWIM likes to leave it go for an extra day or two so you  definetly have a product containing no lactone and everything gets reacted etc. Most of the stuff will react in about 18 hours , so if you wanted to steal a little from the pot then let the rest keep reacting to completion then you should wait a day or so after starting before doing so...

Much credit goes out to c610n2o2 who originally designed and formulated the recipe.  If anyone has any questions or if there is enough interest I will put it up on a/my website...maybe even make a diagram/illustration and extensive commentary...of course if the lycaeum is interested in hosting such a page as well, I'd be Honored if murple or someone at the lycaeum or erowid put it up!!

Thanks all and let me know any comments etc.!

Mike
(RockTheShow@aol.com)

[StraightEdge]

I remember asking a long time ago if this would work, but attempted only a short reaction time (30 mins or something), and it didn't work.

Then what is the rationale behind

Post 294049

(Chromic: "Rxn time", Methods Discourse)?

There's a faster way to get rid of all the lactone. Use NaOH as usual but boil until bubbling stops. You are left with the solid form of NaGHB.

Supposedly the yields with the baking soda method are better.

[Chromic]

The key was that this reaction will not work without water!

With 4 parts water the reaction goes fast with sodium bicarbonate. Try it!!! You'll love it. You'll be as high as I am right now.    I'd post this info to alt.drugs.ghb, but I don't know how to do it anonymously.

Btw: GBL + baking soda does not react. GBL + sodium hydroxide also does not react (?). GBL and a small amount of water plus baking soda (as originally called for in the post above also reacts very slowly, but GBL plus wet sodium hydroxide will react quickly)

[StraightEdge]

Right.....I originally learned from the Chem-R-US synth(NaOH + GBL), which says to add water to both reactants before combining them.

I'll ask my friend to try the baking soda procedure; she will report back to me soon.

[StraightEdge]

NaOH is soluble in (? degrees C) water at 111g per 100ml. Baking soda is soluble in 21C water at a rate of 8.6 grams per 100ml. She usually dissolved the 30 grams of NaOH in 80mL water. Otherwise it would take too long to dissolve. So she made it so that it was at around 1/3 of the saturation point, by mass.

Baking soda is much less soluble than NaOH so she decided to shoot for 1/2 of the saturation point (to avoid using so much water). That would be 4.3 grams per 100mL. Then she found out that Sodium Carbonate, which is soluble at 45.5 g(26 g Carbonate ion) per 100mL in hot water, would be formed when an aqueous solution of Sodium Bicarbonate was heated. Half of the saturation point by mass would be around 13 grams Carbonate ion per 100mL. She was not sure how to convert this into grams of Sodium Bicarbonate added at the beginning. But she hypothesized with the help of

Post 283622

(Chromic: "Re: GHB synthesis - a must read", Methods Discourse) that for every Bicarbonate ion there would only be half as many Carbonate ions (and roughly half as much mass of those ions) around after the water had been heated. The Bicarbonate ion is 61 grams per mole. The Carbonate ion is 60 grams per mole. If 61 grams worth of Bicarb ions are put in that will result in about 30 grams of Carb ions after the water is heated. So to reach the point of half solubility (by mass) she would put in 26 grams per 100mL of Bicarbonate ion. This works out to about 36 grams of Baking Soda per 100mL. To achieve 1/3 saturation, it would be 23 grams per 100mL.

A crockpot was not used as she was not making beef stew. She always tries to use the proper equipment for a job.

22.5g Sodium Bicarbonate (84g/mol divided by 86g/mol, times 23g lactone)
21.9mL lactone originally 20.5mL (23g/1.125g/ml) but added 1.4 for good measure
100mL Water

This is her report:

Baking soda was dissolved in water and heated to 100C. Bubbling (decomposition of Bicarbonate) began at 35C and slowed at 85C. A good amount of excess baking soda had deposited on the bottom of the beaker and did not dissappear until 85C. The solution became clear at this point. It had previously been cloudy. When temperature reached 100C GBL was added. The bubbling seemed to be about 10% of the intensity of that witnessed during previous NaOH reactions. The solution was boiled down until temperature reached 210C (that's what it has registered as on two different thermometers during numerous reactions, either they are broken in exactly the same way or the temperature was that high) and most of the bubbling had stopped. During the boiling down the solution had become cloudy again. The reason for this might be that not all of the Sodium Carbonate had reacted, and it precipitated as the water boiled off because it was insoluble in melted NaGHB. A crude melting point test was done by dipping the thermometer in hot solution then removing it and noting the point at which crystals began forming. This was pretty consistently 120C. In NaOH reactions it was somewhere around 135C although it is difficult to remember. Melting point data for NaGHB could not be found as chemfinder.com is down. At this point the beaker was removed from heat and left to cool. Product was poured into a glass baking pan at 155C. Texture of liquid was smoother than that from NaOH reactions. Texture and color of solid are exactly the same as that of NaOH product.

She's not sure how to properly calculate yield. Before she had added grams of NaOH to grams of GBL to get theoretical yield. But she doesn't know whether that was correct. Nevertheless, for comparison purposes, using that method she got yields of around 95%. In those reactions she used a ratio of 2mL (not grams) GBL to 1g NaOH. Extrapolating from that would tell you that in this new reaction, the theoretical yield would be 35.6g ((21.9*1.125)+(21.9/2)). The actual yield is therefore 91%, which is pretty impressive considering the extra 1.4mL lactone probably didn't even get reacted with. If you exclude that 1.4mL then the yield is 98%. Some of that weight is probably sodium carbonate, but she's not sure how much.

She says she is happy with this procedure and will continue using it from this day forward. She thinks that there may be up to 5% sodium carbonate in the product which she will try to reduce in the future (ingestion is listed as slightly toxic in the MSDS and it is not commonly used in products meant for ingestion).

Be careful once you have decomposed the baking soda. Sodium carbonate is not NaOH, but it is still a strong base.

[StraightEdge]

Throughout the entire process (which took as little time as an NaOH reaction, by the way), there was a one inch band of sodium carbonate precipitated around the top inside edge of the beaker. It first appeared when the decomposition of baking soda began. It seemed like the bubbling had splattered some of the solution on the side of the beaker. The water was driven off leaving sodium carbonate. Some extra water was poured down the sides in an attempt to redissolve this precipitate but it reappeared soon after. The next time the beaker was swirled (after heating to 210C) some of sodium carbonate the was washed from the sides. There was no more lactone left to react with so the melted NaGHB turned cloudy because of the excess sodium carbonate.

There are solutions to this problem. The best would be to use a reaction vessel that is almost closed a the top (a flask) so that it can be swirled more briskly without fear of a spill. Otherwise the last 5mL or so of lactone should be diluted with water, heated, and poured down the sides of the beaker so as to react with the precipitated carbonate.

[Chromic]

The fastest way to complete this reaction is to set your element on max and boil the distilled water and baking soda in a clean saucepan until the conversion to sodium carbonate is done (the little bubbles stop and baking soda is gone), take it off the element, add the GBL and put the lid on, and put it onto an element on minimum heat until the GBL is converted (the lactone smell goes away) which is usually done in 30 minutes.

I haven't seen that build up of sodium carbonate you're talking of... but I have only performed this method about 4 times... I'm glad a few people have tried this out.  

[StraightEdge]

My procedure is not the fastest; but I think it is the fastest for getting a solid product. Most people seem to want the liquid form.

Was your solution ever cloudy at the end of the reaction?

[Chromic]

No, it has never been cloudy. Once I didn't carefully scrub a pot and the solution came out a light brown (though I suppose this doesn't count).

To get solid, I've always just heated until 150C then poured onto aluminum foil. It works like a charm......

[whig]

It should be as easy to acquire washing soda (Sodium Carbonate) directly.

[Chromic]

Washing soda isn't food grade, it's intended for laundry machines. I'm almost sure that it's just as clean, but, why risk it when good quality, nearly pure baking soda is available? I really, really want someone to post this method in alt.drugs.ghb, does anyone know how to do this anonymously (or could tell me how to do it?)?

[whig]

This process is even easier than it sounds.

The molar weight of GBL and NaHCO3 are relatively close, 84g and 86g respectively.  But comparing them by volume, a mL of GBL weighs approximately 1.125g, and a mL (dry) of NaHCO3 weighs approximately 1.167g.

Next, the molar weight of NaGHB is 127g, so with this in mind we can proceed to calculate the proper inputs to obtain a desired output.

SWIM wanted to make 50g of NaGHB powder.  50g NaGHB * 86 / 127 = 34g of GBL, and 34g / 1.125 is 30mL of GBL by volume.  Similarly, 50g NaGHB * 84 / 127 = 33g of NaHCO3, and 33g / 1.167 is about 28.25mL of NaHCO3 by volume.  Since his objective was to ensure that all the lactone was reacted, a tiny bit of extra baking soda would ensure that the end result, tho somewhat basic, would be satisfactory.

Into a pyrex glass vessel he put two level tablespoons of baking soda, and just 100mL dH2O.  Too little water will slow the reaction, he says, but using excessive water just means more time boiling it off later.  He advises that a good rule of thumb here is to double the number of grams being produced and use this many mLs of dH2O.

He placed the vessel on a heating element and set it to max, causing it to be stirred for about a half an hour until it went into clear solution.  Removed from heat, two tablespoons of GBL were then added to the vessel, and it was then placed back onto LOW heat.  Note that too much heat at this point can cause the reaction to be more exothermic than desirable.

After an hour being stirred and kept covered as much as possible (in order to reflux any evaporating lactone back into the vessel), the contents again went clear.  Another half hour of heat and stirring ensured that the reaction was thorough.  This could all be made very simple if one had a heating element with a magnetic stirrer, one might casually read a book while glancing at the reaction from time to time.  If one wanted to do this, it is important to ensure that whatever one used to cover the vessel were not firmly affixed but loosely set on top to allow CO2 and steam pressure to escape.  SWIM does not think anyone wants exploding glassware.

Again he removed the vessel from heat, and allowed it to cool.  In attempting to cool it down he swirled it around a bit and some GHB precipitated causing the contents again to become cloudy.  This was not of concern.  When they were cool enough, a bit was poured off, cooled to room temperature and pH was tested, then this was poured back into the flask and vinegar was added, this process repeated until pH reached around 7.5.

Vessel was again heated until cloudiness dissipated and the contents were again clear.  On another heating element was placed a pan, lined with several layers of aluminum foil forming wide and shallow depression in the middle.  Vessel was poured into lined pan, and heat was applied until boiling recommenced.  SWIM says it is important to not use too much heat or the GHB will scorch.

While evaporation took place, contents were occasionally swirled around to keep an even distribution around the foil depression.  Eventually contents dried and hardened.  At this point was a simple matter to remove foil from pan, and carefully crinkle/separate salt fragments from foil.  He then placed fragments in a coffee grinder, and 50g of NaGHB salt was then poured out into a storage container.

SWIM summarizes as follows:

To make X grams of NaGHB, you need X * 0.6 mL of GBL, X * 0.6 mL (dry) of NaHCO3, and X * 2 mL of dH20.  No simpler process could possibly be imagined.

What a wonderful dream.