Post 440288 (https://www.thevespiary.org/talk/index.php?topic=11864.msg44028800#msg44028800)
(Barium: "PTC - imine reduction", Novel Discourse) with very low yield for mdma and also tried thePost 458857 (https://www.thevespiary.org/talk/index.php?topic=11864.msg45885700#msg45885700)
(Barium: "Improved "wet" reductive alkylation", Novel Discourse) with 0% yield for mdma. Have also heard of other bee's similar findings via pm's. Try Labtops non wet amination.oh thanks for pointing that out, SWIM think 25mg was mistaken as 25g, in the sodium borohydride addition part, thus forming a concentrated base solution.
Yes I'd most definately say that it would kill the reaction! In fact i'd be suprised if you did manage to pull of the reaction with an error like that. With an enourmous amount of heavily polar ions present in the water phase your IPA becomes insoluble, thus forming two layers. The borohydride will dissolve in the water layer, effectively preventing it from reducing the immine. The immine would most likely become much more unstable in the presence of such an amount of base. Overall I would guess that you reduced most of your MDP2P to MDP2Pol (the brown gunk left after stripping the IPA).
Next time, please try a new reaction on a small scale first to prevent bloopers ;)
Regards
Bandil
When stirring was stopped, there were 2 layers formed again, this time the bottom layer(thought to be water) was transperant yellow and the top one(IPA phase) looked very dark. SWIM believe that his water contained too much NaOH and methylamine.hcl added, but all were followed to the letters in this dream.
anyway, swim proceed to add acid to make it acidic and suddenly, the dark color spread to the yellow water. SWIM went on to trip the IPA and the whole mixture looked dark after IPA's absence.
It's quite normal to have two layers after the addition. There are loads of salt present in the water phase, which can make the IPA:water insoluble.
In about 50% of the amination runs I too get a dark IPA:water phase. Especially after the evaporation of the IPA. Very strange indeed; I havn't figured out when out goes dark and when it does not. However, the dark colour is easily removed by washing with DCM or toluene after the IPA has been stripped. Yields also seems unaffected when it goes dark!
I don't see where you get that salt you are talking about? How do you perform the workup? I always acidify and dilute the IPA with water, strip most of the IPA. Then the acidic water:product phase is washed three times with a proper NP (usually DCM). This leaves a perfectly clear water phase, which is basified to give the water white product. After an extraction and subsequent evaoporation with the NP, a white oil is left. This is the very pure end product. So I don't see where you should get salt and brown gunk? Sounds a bit strange to me!
Regards
Bandil
Post 513755 (https://www.thevespiary.org/talk/index.php?topic=10164.msg51375500#msg51375500)
(Bandil: "Easy preparation of HCl salt w/o gassing", Newbee Forum) .Distilled twice uner atm pressure, did not improve much.
Bad idea! You'll get massive degradation of you'r MDP2P at the distillation temperature. Aspirator vacuum will suffice - but please do not distill it at atmospherical pressure.
Regards
Bandil
ended with 0% yield(molar). The solution always turned dark with fast addition. Anyway, SWIM has not got any yield at all so far,
Geez, wasting all that MDP2P! Why not prepare a solution of anhydrous methylamine freebase in methanol? It is simple to do. Then you could use the standard almost dry method and get 90% conversion of your MDP2P into MDMA.