HRID49533

反应详情

EQUATION

反应方程式

HRID 49533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1.00 g of 5-(2-bromo-2-carbamoylethyl)-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide were added 80 ml of tetrahydrofuran and 368 mg of potassium thioacetate under an atmosphere of argon, and the mixture was stirred for 6 hours at room temperature. Solvent was distilled off under reduced pressure, and ethyl acetate was added to the residue, which was washed with water and saturated brine in sequence and dried over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the residue obtained was crystallized from hexane-ethyl acetate, then the crystals were collected by filtration to obtain 904 mg of 5-(2-acetylthio-2-carbamoylethyl)-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide as light brown crystals.

WORKUP

后处理

  1. distillationSolvent was distilled off under reduced pressure, and ethyl acetate
  2. additionwas added to the residue, which
  3. washwas washed with water and saturated brine in sequence
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationSolvent was distilled off under reduced pressure
  6. customthe residue obtained
  7. customwas crystallized from hexane-ethyl acetate
  8. filtrationthe crystals were collected by filtration