HRID2263240

反应详情

EQUATION

反应方程式

HRID 2263240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (14.7 ml, 105 mmol) was added to a solution of 1-(tert-butoxycarbonyl)piperazine (5.64 g, 26.3 mmol) and 5-chloro-3-(2-fluorophenyl)-1,2,4-thiadiazole (4.89 g, 26.3 mmol) in N,N-dimethylformamide (100 ml), the mixture was stirred was stirred at room temperature for 30 minutes, the reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with water, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of hexane and ethyl acetate to give 6.28 g (65.6%) of the desired product as a crystal.

WORKUP

后处理

  1. stirringwas stirred at room temperature for 30 minutes
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was recrystallized from a mixed solvent of hexane and ethyl acetate