HRID2292001

反应详情

EQUATION

反应方程式

HRID 2292001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl thiosalicylate (0.67 g; 0.004M) in 20 ml of methanol is added solid sodium methoxide (0.65 g; 0.012M; 3 eqv.) followed by N-[(3-trifluoromethylphenyl)methyl]-chloroacetamide (1.0 g; 0.004M) and the mixture is refluxed under a nitrogen atmosphere for 30 minutes. The mixture is cooled to room temperature and added to a solution of 1.5 ml of glacial acetic acid in 25 ml of water and cooled to 0° C. The cream colored solid is collected, washed with 50% methanol-water, air dried, and recrystallized from nitromethane to give 1.05 g (78% yield) of the title compound; m.p. 139°-141° C.

WORKUP

后处理

  1. temperaturethe mixture is refluxed under a nitrogen atmosphere for 30 minutes
  2. temperaturecooled to 0° C
  3. customThe cream colored solid is collected
  4. washwashed with 50% methanol-water, air
  5. customdried
  6. customrecrystallized from nitromethane