반응 #310685

반응 방정식

1,1-dimethylethylenediamine

phenylacetyl chloride

→

1,1-dimethyl-2-(2-phenylacetamido)ethylamine

수율 63.7%

용매

ether

ether

반응 조건

후처리

1. 1
   기타The solid was separated by filtration
2. 2
   workup.DISSOLUTIONdissolved in warm water (150 ml.)
3. 3
   기타The solution obtained
4. 4
   여과was filtered
5. 5
   workup.ADDITIONThe filtrate was basified by addition of an excess of saturated aqueous sodium carbonate solution (50 ml.)
6. 6
   추출extracted with chloroform (3×250 ml.)
7. 7
   건조The extracts were dried (MgSO4)
8. 8
   기타evaporated
9. 9
   기타to give an oil which
10. 10
    기타crystallised on addition of a 1:1 v/v mixture of ether and petrol (60°-80°)

실험 절차

A solution of 1,1-dimethylethylenediamine (8.8 g.) in ether (250 ml.) was added during 2 hours to a stirred solution of phenylacetyl chloride (15.4 g.) in ether (250 ml.). This mixture was further stirred for 2 hours. The solid was separated by filtration, and dissolved in warm water (150 ml.). The solution obtained was filtered. The filtrate was basified by addition of an excess of saturated aqueous sodium carbonate solution (50 ml.), and then extracted with chloroform (3×250 ml.). The extracts were dried (MgSO4) and evaporated to give an oil which crystallised on addition of a 1:1 v/v mixture of ether and petrol (60°-80°) to give 1,1-dimethyl-2-(2-phenylacetamido)ethylamine (13.1 g., 63%), m.p. 47°-48° C.

출처