Synthesis of MDE Using Ethylamine

Procedure

180 ml 70% ethylamine was poured into 1qt cold IPA + MeOH (75%, 25%). MgSO4 + NaSO4 was added to the solution to remove all water. The drying agents were then decant off after several hours of falling to the bottom.

50g al was put in a 2liter flask with 1.5 litre clean IPA and allowed to amalgamate for 25 minutes with 400mg HgCl2. After which the 1.5 litre was discarded and replaced with the 700ml ISA and 300ml MeOH along with the 1 litre EtNH2 mix. It was heated for 5 minutes until warm and 95ml of undistilled ketone was dripped in while the reaction was heated by the hotplate at an increasing rate over 20 minutes. There was quite a few problems getting the stirring going; during the first 50 minutes at least 1/2 of that time was spent trying to get the stirring going again. It got so bad that the solution had to be dumped out in a large beaker in a better attempt to use a more suitable container for stirring. It was useless and only fucked things up more, half of the al clung to the bottom of the flask became exposed to raw air for a good 3 minutes during that time and lots of al fell on the floor instead. Finally after 1 hour of fighting it gave in and stirred well; ONLY on a Cole Parmer 6x6 Magnestir of which no piece of shit Corning could seem to handle. The reaction was run for a total of 3.5 hours from start of drip till the end of stirring. Dry Sodium hydroxide was intermitenly added to the stirring reaction to speed it up. It was intended to run for 5 hours but the ol' bat had to come over my house calling me and asking to account where swim was, realizing that he was probably up to his old tricks again.

The unreacted al was filtered off and washed with MeOH, basified the mix, no sludge since tons of unreacted aluminum. Extracted with 1.75 litre toluene and washed several times.

Crystallization:

This part was really cool as it states that crystallization of mdea is so easy you really doubt what you have is legit. 60ml hcl was added until red, decanted off onto a preheated plate and slowly allowed to evaporate under a fan, reheated, fan, reheated, etc. At the point it got down to 50ml volume it was decided to check the consistency of the syrup at room temp. Well, while the stuff was cooling from almost boil to just under hot, no kidding, in less than 2 seconds, the whole liquid hardens so hard so fast that it actually epoxied itself (so to speak) to the pan where it had to be pried off with a flathead screw-driver. And despite it being able to hold massive amounts of water it still crystallized while hot!

The resulting chips (looking like hardened paint) are still pink sandstone color and need recrystallization. Its estimated that ~25-30% is going to be dead weight. Resulting total was 42g impure boulders expected to become 30g after cleanup.