HRID1591743

反应详情

EQUATION

反应方程式

HRID 1591743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.0 g (6.28 mmol) of tert.-butyl N-methyl-β-alaninate, 1.54 g (6.28 mmol) of 2,3-dichlorobenzenesulphonyl chloride and 0.70 g (6.92 mmol) of triethylamine in 30 ml of tetrahydrofuran was stirred at room temperature overnight and then evaporated to dryness. About 50 ml of water were added to the residue, and the mixture was extracted three times with in each case 20 ml of ethyl acetate. The organic extracts were washed with about 20 ml of saturated sodium chloride solution and then evaporated to dryness. The crude product obtained in this manner was purified by column chromatography on silica gel (mobile phase: dichloromethane).

WORKUP

后处理

  1. customevaporated to dryness
  2. additionAbout 50 ml of water were added to the residue
  3. extractionthe mixture was extracted three times with in each case 20 ml of ethyl acetate
  4. washThe organic extracts were washed with about 20 ml of saturated sodium chloride solution
  5. customevaporated to dryness