HRID1358233

反应详情

EQUATION

反应方程式

HRID 1358233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A suspension of 220 mg (0.75 mmol) 2-(2-methoxy-5-morpholin-4-yl-phenylamino)-2-thioxo-acetamide in 2.88 ml 1N aqueous sodiumhydroxde was added to a solution of 813 mg (2.47 mmol) potassium ferricyanide in 2 ml water. The mixture was stirred at 50° C. for 30 minutes and then at room temperature overnight. The precipitate was separated by filtration, dissolved in dichloromethane and purified by column chromatography on silicagel with ethyl acetate/hexane 1/1. 4-methoxy-7-morpholin-4-yl-benzothiazole-2-carboxylic acid amide, 32 mg (15%), was obtained as yellow crystals with mp.: 228-230° C., MS m/e (%): 294 (M+H+, 100).

WORKUP

后处理

  1. customat room temperature
  2. customovernight
  3. customThe precipitate was separated by filtration
  4. dissolutiondissolved in dichloromethane
  5. custompurified by column chromatography on silicagel with ethyl acetate/hexane 1/1