HRID1974345

反应详情

EQUATION

反应方程式

HRID 1974345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (1.0 gram; 0.00968 mole) was added to 3.0 grams of 4-chloro-5,7-dinitro-2-trifluoromethylbenzimidazole (0.00968 mole) in 200 milliliters of benzene. There was then added dropwise 0.8 gram of piperidine (0.00968 mole) in 10 milliliters of benzene. The resulting reaction mixture was refluxed overnight, cooled, an amount of ether added, and the mixture filtered. The filtrate was evaporated, yielding the desired 4-piperidino-5,7-dinitro-2-trifluoromethylbenzimidazole product as an orange solid. It was recrystallized from benzene as a light brown solid, m.p., 199°-206° C. NMR analysis confirmed the identity but suggested the presence of a small amount of triethylamine.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed overnight
  3. temperaturecooled
  4. filtrationthe mixture filtered
  5. customThe filtrate was evaporated