HRID36877

反应详情

EQUATION

反应方程式

HRID 36877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3-Chloropropylsulfonyl chloride 1 (30.28 g,0.17 mol), O-benzylhydroxylamine hydrochloride (27.3 g,0.17 mol), potassium carbonate (50 g,0.36 mol) and tetrabutylammonium sulfate (about 500 mg) are reacted with each other in a mixture of ether and water (1:1) (100 ml) for 24 hours at room temperature and the reaction mixture was extracted with ethyl acetate. The extract was subjected to column chromatography on silica gel. From the fraction eluted with a mixture of ethyl acetate/n-hexane (1:4),18.4 g (41%) of crude N-benzyloxy-3-chloropropylsulfonamide (intermediate 3g) was obtained as a pale yellow oil.

WORKUP

后处理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washFrom the fraction eluted with a mixture of ethyl acetate/n-hexane (1:4)