HRID2263073

反应详情

EQUATION

反应方程式

HRID 2263073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-(3,4-dimethylisoxazol-5-yl)piperazine-1-carboxamide trifluoroacetate (297 mg, 0.707 mmol), 5-chloro-3-(2-fluorophenyl)-1,2,4-thiadiazole (152 mg, 0.707 mmol), triethylamine (0.491 ml, 3.53 mmol) and N,N-dimethylformamide (3 ml) was stirred at room temperature for 0.5 hours, 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 tetrahydrofuran and ethyl acetate to obtain the desired product (44.0 mg, 15.5%) as a solid.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was recrystallized from a mixed solvent of tetrahydrofuran and ethyl acetate