HRID275842

反应详情

EQUATION

反应方程式

HRID 275842 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of N-methyl-N-methyloxy-2-amino-5-chlorobenzamide (2 g) and 2-(3-bromophenyl)-1,3-dioxolane (2.1 g) in tetrahydrofuran (65 ml) was cooled to −78° C. To the solution was added dropwise gradually a hexane solution of n-butyl lithium (1.6 mol/L)(11.6 ml). To the mixture were added water (300 ml) and acetic acid ethyl ester (50 ml). The organic layer was washed with water and dried over anhydrous Na2SO4, then the solvent was distilled off. The residue was purified by means of a silica gel column chromatography to give 2-[3-(2-amino-5-chlorobenzoyl)phenyl-1,3-dioxolane (1.6 g) as a colorless oily compound.

WORKUP

后处理

  1. washThe organic layer was washed with water
  2. dry with materialdried over anhydrous Na2SO4
  3. distillationthe solvent was distilled off
  4. customThe residue was purified by means of a silica gel column chromatography