HRID866780
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
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
- temperatureThe mixture was heated
- temperatureat reflux for one hour
- filtrationthe dibenzylamine hydrobromide was filtered
- customdried
- temperatureto cool
- customwhen the crude product crystallised
- filtrationThis was filtered off
- customdried
- customrecrystallised from ethyl acetate, (5 l)