HRID2290185

反应详情

EQUATION

反应方程式

HRID 2290185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred solution of 5-bromo-6-methylsulfamoylindoline, 55.92 g (0.19 mol) in 150 ml dioxane was added 41.79 gm (0.184 mol) of 2,3-dichloro-5,6-dicyanobenzoquinone at 25° C. The resulting brown solution was heated to 80° C. for 2 hours when thin layer chromatography using chloroform showed that the reaction was complete. The reaction mixture was allowed to cool, filtered through Celite and the filtrate concentrated under reduced pressure. The resulting brown solid was stirred in a mixture of methylene chloride/ether 50/50 and then filtered. This procedure was carried out two additional times and gave 35.2 g (63.9% by weight yield) of 5-bromo-6-methylsulfamoylindole.

WORKUP

后处理

  1. temperatureto cool
  2. filtrationfiltered through Celite
  3. concentrationthe filtrate concentrated under reduced pressure
  4. filtrationfiltered