The One Pot d,l-Meth and ICE.
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LaBTop .......... posted 06-23-99 01:04 PM
Member

Making of d,l-Meth ice(cream).

Ingredients:
• 138 gram P2P = +/- 1 grammole.
• 1000 ml Methanol (+ 10 % weight Methylaminegas)= +/-3gmol.
• 36 gram MgSO4.7H2O (dry at 300 C for 2 Hrs in oven to get MgSO4.1H2O)=to attrack 2 gmol H2O.
• 200 ml Silicagel balls +/- 3 to 5 mm (dry at 300 C for 2 Hrs in oven, changes to dark brown! ).
• 15 gram NaBH4 as a reducing agent for the formed (waterfree !) Imine.

IMPORTANT: THE REACTION IS VERY SENSIBLE FOR ANY WATER (fluid or vapour in the air!).

First quickly crunch your DRY MgSO4 to a powder in a mortar, and directly put that under max. mixing in the Methanol/M.A. mix and close the pot to let no water from the air in. Keep mixing for 10 minutes, then all the water will be taken up to the MgSO4. Let stand and wait till all the MgSO4 is on the bottom. Now quickly tap off the now DRY MeOH/MA mix in 2L reaction flask and close that one. Wash directly your empty pot with lots of water, to remove the smell of methylamine! Now add the 200 ml DRY Silicagel balls and a magnetic mixer bar also in the flask and close again. Keep 2L flask in Silicone-oil bath at 20 C. Silicone-oil only slowly warms up! Now add SLOWLY via a dropping funnel the 138 gr P2P to the 2L flask under strong mixing. The temperature rises to 23 C during the waterfree Imine forming. The water from this reaction is taken up by the dried Silicagel! This takes 30 minutes. Let then mix for another 1 hour. The reactionmix color changes from light yellow to coffee+milk color. Temp= 23 C. Stop mixing after this 1 hour and pour the fluid off into a 2L glas erlenmeyer with flat bottom and add a mixbar. The remaining Silicagel is washed 3 times with 50 ml DRY methanol, to catch the remaining Imine, and those 2 x 50 ml is also poured into the 2L erlenmeyer. Now put the 2L em on magn.mixer, in a icecubes/methanol bath and start strong mixing. Put a Funnel on top of 2L em, in rubber ring. Now start adding, every 5 min., a teaspoonfull (flat off!) of boro and wash in with minimum methanol. After every spoonfull, stopper the funnel loosely with a rubber stopper. This takes 2,5 hrs. DO NOT exceed a temp of more then 20 C !! You can add the next spoon at +/- 8 C. Solution color is light clear orange/brown. Let mix in total for 8,5 hrs.(could perhaps be lot less hours, do'nt want to know: time is NOT money!) The total volume is +/- 1900 ml. Add then the mix to 5 L dest. water in a 10 L flask, under magn.mixing. The pH=12 . Add then 500 ml diChloromethane (DCM) and mix strongly for 30 min. Let oil precipitate and a dark,honey-coloured layer of DCM+oil is on the bottom. Decant the waterpart with a aspirator+siliconetube. Fill the rest (water+DCM+oil) in a seperator funnel and tap off only the DCM+oil=550 ml. (DCM boiling point=40 C). The leftover MgSO4 and boro salts stayed nicely in the waterpart. Then dry the DCM+oil with some DRY MgSO4 and decant in 2L em. Wash this MgSO4 with some fresh, DRY DCM and add the DCM washings to the now dry DCM+oil. Total volume DCM+oil =1000 ml, colour is honey/red. Start now bubbling this 1000 ml with HCl-gas, while 2L em stands in icebath on magn.mixer and mix strongly. Check pH frequently, until pH 6. Pour the now acidified 1000 ml in a 2 L evap.flask and put on Rotavap machine. Speed= 100 rpm , temp= 80 C, mode=p/auto, little vacuum=800 mbar, to hold the flask. After distillating off nearly all the DCM, suddenly the contents of the flask turns from dark honey colour to creamy milk color and it dries out to a round cake on the bottom. Remove the 1 L DCM, now in the collector flask, and hang that empty flask on again. Now put full vacuum on to remove the last traces of water. Cleaning by 3 x recrystalization: Put MINIMUM quantity of hot (40 C) DRY DCM (or dry 98+% Ethanol) in the flask until the last remains of the dry stuff dissolves, and add 4 x this DCM-quantity as DRY acetone. Close with stopper and put 1 hr in freezer. A solid dirty-white crystal mass is formed with a layer of dark red fluid on top of it. Decant the fluid and repeat this step another 2 x and 2 Hrs. You have, the last time, snow white crystals. Dry Weight = 141,5 gram, close to quantitative yield. You can eventually melt this crystal mass in a alu flatbottom pot on a heaterplate at 170-175 C. Then let this melt VERY SLOWLY, and do not go higher then necessary to melt it, or its starts smoking ( you have your first quick-test then: enjoy!). Cool down to 150 C again, really slowly, 1 degree C per 30 min. (regulate with your temp controller!), and you got d,l-ICE, after you let it very slowly again cool down to roomtemperature (with a closed lid on it!, its hygroscopic ! ). Advantage: you removed ALL the water in this process!!!

So now you know at last how to make ICE cream....... Ravers LOVE it!!!! LT/

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EMOTIONSwill always beFREE!

LaBTop .......... posted 06-23-99 01:19 PM
Member

Yohoo, forgot to tell:
Use d-Tartaric acid to get d-Meth !!!!!!!!
2 Flies in one hit....

Ask your beloved moderator, the unforgettable MR Spit_tartar_Ball, how to do that, he recently posted the method, but needs a little explaining for most of you, I'm afraid. But thou should NOT be afraid, its easy!

Then you have d-Meth AND l-Meth (speedy only). Life becomes easier and easier......? LT/