反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solid was separated by filtration
- dissolutiondissolved in warm water (150 ml.)
- customThe solution obtained
- filtrationwas filtered
- additionThe filtrate was basified by addition of an excess of saturated aqueous sodium carbonate solution (50 ml.)
- extractionextracted with chloroform (3×250 ml.)
- dry with materialThe extracts were dried (MgSO4)
- customevaporated
- customto give an oil which
- customcrystallised on addition of a 1:1 v/v mixture of ether and petrol (60°-80°)