HRID866780

反应详情

EQUATION

反应方程式

HRID 866780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Bromoacetyl salicylamide (515 g) was added to a stirred solution of dibenzylamine (750 g) in ethyl methyl ketone (3.0 l). The mixture was heated at reflux for one hour and the dibenzylamine hydrobromide was filtered and dried. The filtrate was allowed to cool, when the crude product crystallised. This was filtered off, dried, and recrystallised from ethyl acetate, (5 l), to give 5-(N,N-dibenzylglycyl)salicylamide as an off-white solid (336 g), m.p. 168°.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for one hour
  3. filtrationthe dibenzylamine hydrobromide was filtered
  4. customdried
  5. temperatureto cool
  6. customwhen the crude product crystallised
  7. filtrationThis was filtered off
  8. customdried
  9. customrecrystallised from ethyl acetate, (5 l)