HRID1354253

反应详情

EQUATION

反应方程式

HRID 1354253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-[2-(5,6-Difluorobenzimidazol-2-ylthio)ethyl]-4-formylpiperazine (1.70 g, 5.2 mmol) was dissolved in methanol (20 mL), and 12N hydrochloric acid (2 mL) was added to the solution, followed by stirring for 18 hours at room temperature. The reaction mixture was concentrated under reduced pressure, and saturated ammonia-methanol was added thereto, followed by stirring for five minutes at room temperature. The solvent was removed under reduced pressure, and the residue was purified through silica gel column chromatography (chloroform: saturated ammonia-methanol=100:3), to thereby yield 1-[2-(5,6-difluorobenzimidazol-2-ylthio)ethyl]piperazine (1.40 g, yield 90%) as a brown oil.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and saturated ammonia-methanol
  2. additionwas added
  3. stirringby stirring for five minutes at room temperature
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified through silica gel column chromatography (chloroform: saturated ammonia-methanol=100:3)