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Topic: KHMDS using  (Read 4988 times)

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Offline marcinosss

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KHMDS using
« on: November 12, 2010, 01:30:43 PM »
Hi,

I'm going to do reaction: Ph2C=NCH2P(O)(OPh)2 + Br(CH2)2CO2CH2Ph  :rarrow:
I want generate anion of Ph2C=NCH2P(O)(OPh)2 using KHMDS.
How should I use KHMDS? I think first I add KHMDS to Ph2C=NCH2P(O)(OPh)2 -78oC, then (past 2h?) I add Br(CH2)2CO2CH2Ph. To end reaction I add NH4Cl. Am I right? Is it necessary using inert atmosphere?

Thanks for any suggestions.

Offline MissPhosgene

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Re: KHMDS using
« Reply #1 on: November 12, 2010, 04:11:39 PM »
Use inert atmosphere and keep the reaction water free. If you don't the end result will probably be a mess.

I would add the phosphonate to KHMDS with an addition funnel instead of the other way around. Make a solution of known concentration which is in excess of what you need, cannula the necessary amount into a dry addition funnel under inert atmosphere and then add that to the base.

Stereograms of the 32 crystallographic point groups: little bike wheels of cold, hard, pure rationality.

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