HRID275857

反应详情

EQUATION

反应方程式

HRID 275857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A tetrahydrofuran (30 ml) solution of N-methyl-N-methyloxy-2-aminobenzamide (2.70 g) and N-tert-butoxycarbonyl-3-bromobenzylamine (2.86 g) was cooled to −78° C. To the solution was gradually added dropwise a hexane solution of n-butyl lithium (1.6 mol/L) (31 ml). To the mixture were then added water (70 ml) and acetic acid ethyl ester (70 ml). The organic layer was washed with water and dried over anhydrous MgSO4. The solvent was then distilled off. The residual oily compound was purified by means of a silica gel column chromatography to give 2-amino-3′-(tert-butoxycarbonylaminomethyl)benzophenone as a yellow oily product (1.2 g).

WORKUP

后处理

  1. washThe organic layer was washed with water
  2. dry with materialdried over anhydrous MgSO4
  3. distillationThe solvent was then distilled off
  4. customThe residual oily compound was purified by means of a silica gel column chromatography