HRID36695

反应详情

EQUATION

反应方程式

HRID 36695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

89 g (0.5 mol) of ethyl N-(2,2-dimethoxyethyl)-carbamate are added dropwise to 17.5 g (0.58 mol) of NaH (80% strength in paraffin oil) in 500 ml of absolute toluene at 80° C. The mixture is then stirred for one hour and 80 g (0.59 mol) of 1-bromo-2-butene are subsequently added dropwise at 80° C. The mixture is stirred at 80° C. overnight and cooled, the salts are dissolved with water and the aqueous phase is separated off and extracted with toluene. The toluene solutions are dried over K2CO3 and concentrated and the residue is distilled.

WORKUP

后处理

  1. stirringThe mixture is stirred at 80° C. overnight
  2. temperaturecooled
  3. customthe aqueous phase is separated off
  4. extractionextracted with toluene
  5. dry with materialThe toluene solutions are dried over K2CO3
  6. concentrationconcentrated
  7. distillationthe residue is distilled