HRID223503

反应详情

EQUATION

反应方程式

HRID 223503 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customThe solid was separated by filtration
  2. dissolutiondissolved in warm water (150 ml.)
  3. customThe solution obtained
  4. filtrationwas filtered
  5. additionThe filtrate was basified by addition of an excess of saturated aqueous sodium carbonate solution (50 ml.)
  6. extractionextracted with chloroform (3×250 ml.)
  7. dry with materialThe extracts were dried (MgSO4)
  8. customevaporated
  9. customto give an oil which
  10. customcrystallised on addition of a 1:1 v/v mixture of ether and petrol (60°-80°)