Author Topic: Strange emulsion and color change in Al/Hg workup  (Read 1919 times)

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TheBlindGenius

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Strange emulsion and color change in Al/Hg workup
« on: June 02, 2003, 03:28:00 AM »
OK, so swim did a reductive amination with 50 g ketone, 50mL 40% aq. methylamine, 25 g foil, etc.  He did it as per Osmium/Brightstar's writeup.  However, when the rxn finished and he basified, he was left with a grey solution.  Great.  Sounds about right.  He added 400 mL clear toluene to the solution and left it stirring for 4 hours (he had to go do something important).  When he came back he had a orangish solution!  No layers!  So he added some salt and shook in a sep funnel.  Now he got a light orange toluene layer, huge oil droplets (emulsion?) in the interface, and a darker orange water layer.  What should he do next?  He is especially confused as to the very noticeable color change.


bones

  • Guest
pink is common when using impure ketone...
« Reply #1 on: June 02, 2003, 07:12:00 AM »
pink is common when using impure ketone... im assumning that perhaps orange is from the same cause...hopefully someone else will give ya more help with that....anyway...asside from the garbage in garbage out rule... you may  still be able to get some honey... take a sample of you toluene layer and gas it... if you dont get anything then start panicing .. wash anything you get really well with acetone.. if your really paranoid consider distilling your amine oil.. not that ive ever done that...

as for your emulsion.. what i'd do here is to tap off your clean toluene layer... after thats gone you can start to worry about the rest... firstly id simply try adding some more toluene... give her a good shake and do all the normal things like swerling and stuff...go have a couple of beers... mabey watch some footy or something (this part is optional) ...if this dont work consider adding a nother solvent missible with toluene.... just a small amount... perhaps DCM... this will disolve the organic stuff.... any will certainly kick out anything aqueous....might be nice to distill it off again before gassing... mdma.hcl is kinda soluable in chloronated solvents .. so you'll loose yeild if ya dont... not sure how much yeild though.

let me know what you get from gassing your orange solution... id really appreciate all the details you could give... color, taste, solubility, rf if you can, etc.. goodluck

TheBlindGenius

  • Guest
It worked out
« Reply #2 on: June 02, 2003, 08:00:00 AM »
swim just added more solvent.  Swim realized the "emulsion" was really just crud, so he filtered it out.  BTW, the solution had been filtered 5 hours prior to this, I guess more crud formed in the time.  Some crud still stayed in the interphase, so just didn't let that get into the toluene layer.  Made sure to let some of the toluene layer get away.  Purity is more important than yield to swim.  Anyways, after gassing, someone's dog got lots and lots of very white xtals.  They stink of toluene though, even after drying in a low-temp oven.  What to do?


bones

  • Guest
wash em with acetone... that seems to help...
« Reply #3 on: June 02, 2003, 08:12:00 AM »
wash em with acetone... that seems to help... if they still smell pear shaped.. consider grinding em and allowing to dry... dont worry.. eventually it'll just have to evaporate...