HRID377664

反应详情

EQUATION

反应方程式

HRID 377664 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 4-acetyl-5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole (0.302 g) in tetrahydrofuran (10 ml) at 2° C. was added t-butylnitrite (0.66 ml). The mixture was heated under reflux for 1.5 hours and then evaporated. The residue was purified by column chromatography on silica gel eluted with dichloromethane. Combination and evaporation of suitable fractions provided the title compound as a white solid, m.p. 105.7-106.6° C.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel
  5. washeluted with dichloromethane
  6. customCombination and evaporation of suitable fractions