HRID1944697

反应详情

EQUATION

反应方程式

HRID 1944697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
67.5 °C

PROCEDURE

实验过程

To a mixture of 2-thioxo-2,3-dihydrobenzooxazole-5-carbonitrile (2.56 g, 14.5 mmol) and thionylchloride (14.1 mL) was added two drops of DMF. The mixture was heated at 65-70° C. for 1 h. Then the mixture was cooled to rt and diluted with CH2Cl2. The solvent and excess thionylchloride were removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: 20% EtOAc in Petroleum ether) to give 2-chlorobenzooxazole-5-carbonitrile 1.69 g (65%).

WORKUP

后处理

  1. temperatureThen the mixture was cooled to rt
  2. customThe solvent and excess thionylchloride were removed under reduced pressure
  3. customThe residue was purified by column chromatography on silica gel (eluent: 20% EtOAc in Petroleum ether)