HRID1079318

反应详情

EQUATION

反应方程式

HRID 1079318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of sodium periodate (3.09 g) in water (25 ml) was added dropwise with cooling to a stirred solution of 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine (2.88 g, prepared in a similar manner to that described in the preceding paragraph) in dichloromethane (75 ml). The stirring was continued at room temperature for 19 hours. Solvent was removed from the mixture by evaporation at reduced pressure. Purification of the residue by flash chromatography using dichloromethane/ethanol (95:5) as eluent gave 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide, which was recrystallised from ethyl acetate. Yield 2.15 g (m.p. 125°-126° C.).

WORKUP

后处理

  1. customprepared in a similar manner to that
  2. customSolvent was removed from the mixture by evaporation at reduced pressure
  3. customPurification of the residue by flash chromatography