HRID2263033

反应详情

EQUATION

反应方程式

HRID 2263033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixed solution of 2,2,2-trichloroethyl (1,1-dioxido-1-benzothien-6-yl)carbamate (257 mg, 0.720 mmol), 1-[3-(2-thienyl)-1,2,4-thiadiazol-5-yl]piperazine (200 mg, 0.792 mmol) and diisopropylethylamine (0.129 ml, 0.720 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 70° C. for 3 hours. Water was poured to the reaction mixture, and the resulting solution 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. Chloroform was added to the residue, and 69.6 mg (21.0%) of the desired product as a solid was separated by filtration.

WORKUP

后处理

  1. extractionthe resulting solution 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. additionChloroform was added to the residue, and 69.6 mg (21.0%) of the desired product as a solid
  6. customwas separated by filtration