HRID2426132

反应详情

EQUATION

反应方程式

HRID 2426132 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3-Chloro-4-fluoro-benzoic acid 5-(3-chloro-4-fluoro-benzoylamino)-2-methyl-phenyl ester (3.93 g, 9 mmol) was dissolved in a mixture of tetrahydrofuran (25 mL), methanol (50 mL) and aqueous 1N sodium hydroxide (9 mL, 9 mmol). The mixture was stirred at room temperature for 18 hours and then concentrated under reduced pressure to remove most of the organic solvent. The resulting suspension was diluted with water (45 mL) and saturated aqueous sodium bicarbonate solution (5 mL). After standing for 30 minutes, the precipitate was collected and washed with water and dried to give crude 3-chloro-4-fluoro-N-(3-hydroxy-4-methyl-phenyl)-benzamide as a white powder. (Yield 2.59 g, 103%).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. customto remove most of the organic solvent
  3. additionThe resulting suspension was diluted with water (45 mL) and saturated aqueous sodium bicarbonate solution (5 mL)
  4. waitAfter standing for 30 minutes
  5. customthe precipitate was collected
  6. washwashed with water
  7. customdried