methlab (Hive Bee)
03-12-04 11:55
No 494680
       Now i know why i never reached expected yield     

I've never reached the expected yield after aminating our favourite ketone, just 1/2 - 2/3 - bad, i know.
I hate it when things like this happen, so i started to check all Al/Hg and post Al/Hg steps. I knew the
'error' must be there. The last two weeks i nerved you guys with questions about methylamine concentration
a.s.o, but everything was ok. Error: I just own a big buchner, which my aspirator could not pull, so i
did NOT use it, just gravity filtration. I was allways wondering why i am loosing so much of the
toluene/freebase mix, but i thought ok that's life (You are allowed to laugh here). Today i thought i should give it another try and i build an inlay for my buchner to narrow the surface area. My water aspirator could handle it now. After gasing, I threw in this sticky
coconutmilklike thing, i thought i'm dreaming, most of the toluene passed the filter ! After three gasings
+ filtering i was left with the expected yield and a lot of the toluene was still there...
OK guys, all together: clap your hands and laugh for a minimum of 10 seconds... Hope there is noone else out there, doing the same mistake as i, but as an excuse, i am just a computer scientist...blush 		 
 
 
 
    homeslice
(Hive Bee)
03-12-04 13:13
No 494685
       i dont understand your post but i wish i did...     

i dont understand your post but i wish i did as i also know someone who only seems to get 2/3 to 3/4 yield
Never take a fox's word that the hens are safe. 		 
 
 
 
    ApprenticeCook
(Hive Bee)
03-12-04 15:25
No 494720
       RIP     

Yeah workup is usually the one that gets you, got to make sure everything is in order. Spose that error was staring you in the face but you didnt see it until the dream was over? hmmm RIP lost honey. 		 
 
 
 
    GC_MS
(Hive Addict)
03-13-04 03:18
No 494830
       ha ha ha ha.... ha ha ha ha     

What really puzzles me is where you found the patience necessary to subject the Al-sludge to gravity filtration smile. I mean, I am known as a very calm and patient personality, but that would just be over the line.

A little tip: use celite for your vacuum filtration. You can read more about it Post 384725 (Chromic: "Celite", Methods Discourse). Better luck next time wink.
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