Success is also guaranteed when using the following directions
...
You will need:
- 1 thermometer capable of measuring at least 160°C
- several pyrex/duran beakers
- 1 measuring jug (accurate to 5 ml)
- 1 digital scale, (accurate to at least 0.1g)
- the notorious pyrex baking dish (or a baking plate covered with aluminum foil)
- big-sized ziploc baggies or air-tight container
and, of course
- gamma-butyrolactone (GBL)
- solid NaOH (preferably ACS grade or food grade if there is any )
- distilled H2O (no tap water please)
1. Weigh out 86.1 g GBL, put in clean beaker and add 20ml H2O to it.
2. Dissolve
exactly 40.0 g NaOH in 100ml H2O.
3. Heat the GBL/H2O mixture to 105°C using a hotplate. Use the thermometer to stir it and to check the temperature. Keep at 105°C for ~10 minutes, while stirring occasionally.
5. turn off the hotplate.
4. Add the NaOH solution
dropwise to the hot GBL/water mixture. Every drop will first go to the bottom and then vigorously react, producing small bubbles (boiling due to exotherm rxn).
5. After having added a certain amount of NaOH, you will see a bottom layer of NaGHB soln. and a top layer of unreacted GBL/GHB. Keep adding NaOH in little squirts, while stirring and monitoring the temp. with the thermometer.
6. When the temp. falls below 90°C, turn on the hotplate again; if it climbs to more than 110°C, remove the beaker until it is around 100°C again. Important is that the temp. is kept between 90-110°C during NaOH addition.
7. Watch the upper layer (it is somewhat cleaner than the lower salt/lye layer): you want to add NaOH solution until it has disappeared completely. So you have to slow down the addition rate as the layer gets next to nothing, and stir vigorously between the single additions. Finally, you will just see a few drops of lactone/hydroxybutyrate on top of your NaGHB solution. Drip in a few more drops of your NaOH - it shouldn't be left much of it by now.
If there is more than 10% left, your GBL wasn't pure, or you weighed incorrectly...
8. Now add 100ml H2O, and set your hotplate to maximum. Boil away the water to steam distill any unreacted lactone, remove eventual impurities derived from the GBL and to complete the reaction. No pH checking while hot/cold whatsoever...
9. The temperature will rise during steam "distillation": if it reaches the 150°C mark, you will want to keep it there; so you must remove the beaker (caution - hot!) from the hotplate and put it back on as it cools down. Continue until no bubbles evolve anymore. You now have a viscous, odorless and slightly yellowish tinted NaGHB melt. If it still smells like GBL ("sour" odor), go back to step 8.
10. Cautiously (hot!) pour the molten NaGHB into your pyrex dish or similar, trying to form strips. It will solidify almost instantly. Let cool a few minutes and scrape together the still warm NaGHB with a spatula, knife etc. If you're careful, you will be able to loosen big plates/chunks at once. Otherwise you'll have to scrape very hard, as it really sticks to the pyrex dish
.
Immediately place the chunks/powder into a ziploc baggie - they are very deliquescent and end up as little puddles if you wait too long...
You now have "crude" solid NaGHB.
(11. (optional))
Weigh out exactly 100 grams of NaGHB, place in beaker, and add enough H2O to give a total volume of slightly less than 200 mls. Heat under stirring until all solids have dissolved, then pour into graduaded measuring jug and adjust the volume to exactly 200ml with H2O.
(you can put a little bit food color into the water you use for volume correction, to give an appealing nice colored NaGHB solution
). You now have 200mls of a nice colored 0.5g/ml NaGHB solution, ready to use, perfect for those handy-dandy 2ml PE pipettes...
If it is done right, the resulting NaGHB solution is neutral (pH 7.5), with a yield of just 95%, due to small lactone losses...
But with this method, it is impossible to add too much NaOH, and impossible to have remaining lactone contaminations as well. The product in solution will in fact be odor- and tasteless! (Promised!)
indole_amine