HRID84635

反应详情

EQUATION

反应方程式

HRID 84635 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 9-bromo-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-2-carboxylic acid ethyl ester (500 mg), potassium ferrocyanide (dried, 104 mg), copper (I) iodide (27 mg) and 1-butylimidazole (0.37 mL) in toluene (3 mL) was reacted in the microwave at 160° C. for 4 h. The mixture was then partitioned between dichloromethane (30 mL) and water (20 mL). The organic layer was dried (MgSO4), reduced in vacuo and purified on silica to give 9-cyano-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-2-carboxylic acid ethyl ester.

WORKUP

后处理

  1. customwas reacted in the microwave at 160° C. for 4 h
  2. customThe mixture was then partitioned between dichloromethane (30 mL) and water (20 mL)
  3. dry with materialThe organic layer was dried (MgSO4)
  4. custompurified on silica