HRID978428

反应详情

EQUATION

反应方程式

HRID 978428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 147 g of 1,4-diaminobutane in 490 ml of methylene chloride, a solution of 41 ml of benzyl chloroformate in 84 ml of methylene chloride was added dropwise at 0° over a period of 1 hour. The mixture was stirred at 0° for 1 hour, then washed twice with water and extracted four times with 150 ml of 4N hydrochloric acid. The acidic extracts were washed with methylene chloride, basified with 450 ml of 22% of sodium hydroxide and extracted four times with methylene chloride. The organic extracts were dried over magnesium sulfate and evaporated to give 4-benzyloxycarbonylamino-1-butylamine, having NMR peaks at δ=7.3, 5.05 and 2.6 ppm.

WORKUP

后处理

  1. washwashed twice with water
  2. extractionextracted four times with 150 ml of 4N hydrochloric acid
  3. washThe acidic extracts were washed with methylene chloride
  4. extractionextracted four times with methylene chloride
  5. dry with materialThe organic extracts were dried over magnesium sulfate
  6. customevaporated