Alright so the old man down the road finally decided to give this a go, heres what I witnessed:
-1.1g MDA.HCl basified, extracted twice with DCM
-DCM stripped off, the remaining base then taken up in MeOH
-To this was added 0.38ml formalin (though I screwed up the pipetting of such a small amount, inevitably this caused an excess)
-The solution of MDA formaldehyde imine was then left in a dropping funnel for ~1hr.
-in an RB, 120mg of HgCl2 (originally started with 20mg, then kept adding more to get a decent reaction rate) and ~0.2g aluminium were amalgamated in a solution of MeOH.
-The amalgam mixture was brought to ~50°c and the MDA formaldehyde imine solution then dripped in.
-Reaction ran for ~2hrs, when most of the aluminium was used up, keeping in mind I used a decent excess of aluminium.
-Reaction volume was doubled using a solution of NaOH, then filtered to remove solids.
-The remaining liquid was extracted twice with xylene.
Yet to do the final work up to get the final result and yield (if any), will post when this is done. This is my first time witih Al/Hg and I must say I already dislike working with HgCl2, its a pain in the ass because of the precautions needed with cleaning etc. Seems like Al/Ga could be used, though im yet to find any good posts regarding its use (if anyone has any, please share).
Reference: http://www.erowid.org/archive/rhodium/chemistry/amphetamine.methylation.html
-1.1g MDA.HCl basified, extracted twice with DCM
-DCM stripped off, the remaining base then taken up in MeOH
-To this was added 0.38ml formalin (though I screwed up the pipetting of such a small amount, inevitably this caused an excess)
-The solution of MDA formaldehyde imine was then left in a dropping funnel for ~1hr.
-in an RB, 120mg of HgCl2 (originally started with 20mg, then kept adding more to get a decent reaction rate) and ~0.2g aluminium were amalgamated in a solution of MeOH.
-The amalgam mixture was brought to ~50°c and the MDA formaldehyde imine solution then dripped in.
-Reaction ran for ~2hrs, when most of the aluminium was used up, keeping in mind I used a decent excess of aluminium.
-Reaction volume was doubled using a solution of NaOH, then filtered to remove solids.
-The remaining liquid was extracted twice with xylene.
Yet to do the final work up to get the final result and yield (if any), will post when this is done. This is my first time witih Al/Hg and I must say I already dislike working with HgCl2, its a pain in the ass because of the precautions needed with cleaning etc. Seems like Al/Ga could be used, though im yet to find any good posts regarding its use (if anyone has any, please share).
Reference: http://www.erowid.org/archive/rhodium/chemistry/amphetamine.methylation.html