HRID275860

反应详情

EQUATION

反应方程式

HRID 275860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A tetrahydrofuran (15 ml) solution of N-methyl-N-methyloxy-2-amino-5-methyloxy-benzamide (0.35 g) and N-tert-butoxycarbonyl-3-bromobenzylamine (0.48 g) was cooled to −70° C. To the solution was added dropwise, while stirring, a hexane solution of n-butyl lithium (1.6 mol/L) (6.2 ml) over 20 minutes. To the mixture were then added water (40 ml) and ethyl acetate (40 ml). The organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by means of a silica gel column chromatography to give 2-amino-3-tert-butoxycarbonylaminomethyl-5-methyloxy-benzophenone as a yellow oily product (0.18 g).

WORKUP

后处理

  1. additionTo the solution was added dropwise
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customThe residue was purified by means of a silica gel column chromatography