HRID1681474

反应详情

EQUATION

反应方程式

HRID 1681474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-methoxy-4-bromoisothiazole (2.9 g, 15 mmol) in methylene chloride (15 ml) there can be was added, in portions, 3,5-dinitroperbenzoic acid (3.4 g, 15 mmol) with ice bath cooling. After about one hour, the precipitated 3,5-dinitrobenzoic acid can be filtered off and the solvent evaporated in vacuo. By triturating the residue with diethyl ether, a crystalline product, 3-methoxy-4-bromoisothiazole-1-oxide, can be obtained. Additional material can be obtained by chromatographing the mother liquors on silica gel, eluting with chloroform.

WORKUP

后处理

  1. temperaturecooling
  2. filtrationthe precipitated 3,5-dinitrobenzoic acid can be filtered off
  3. customthe solvent evaporated in vacuo
  4. customBy triturating the residue with diethyl ether