HRID280637

反应详情

EQUATION

反应方程式

HRID 280637 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-(4-chlorobenzoyl)benzyl bromide (4.2 g, 13.6 mmol) and sodium azide (1.32 g, 20.3 mmol) in ethanol (40 ml) was refluxed for 5 hours, cooled to ambient temperature, and kept 16 hours. The mixture was filtered and the solids were washed twice with ethanol. The combined filtrate and washes were evaporated to dryness under vacuum and the residue was treated with diethyl ether and filtered. The filtrate was evaporated to dryness under vacuum and dried to provide 3.7 g (100%) of 3-(4-chlorobenzoyl)-benzyl azide, m.p. 43°-45° C.

WORKUP

后处理

  1. temperaturewas refluxed for 5 hours
  2. filtrationThe mixture was filtered
  3. washthe solids were washed twice with ethanol
  4. customThe combined filtrate and washes were evaporated to dryness under vacuum
  5. additionthe residue was treated with diethyl ether
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness under vacuum
  8. customdried