HRID657333

反应详情

EQUATION

反应方程式

HRID 657333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a suspension of 3-bromo-5-(methyloxy)benzoic acid (9.6 g, 41.6 mmol) in toluene (60 mL) were added thionyl chloride (9.89 g, 83.1 mmol) and DMF (0.10 mL) and the mixture stirred at 50° C. for 4 h. The mixture was allowed to cool to room temperature, and then the excess thionyl chloride was removed in vacuo. The residue was dissolved in toluene (50 mL), and the mixture was added to a solution of ammonia (25%, 50 mL). A precipitate formed and was filtered off using Celite, and dried to afford 3-bromo-5-(methyloxy)benzamide (8.70 g, 90%).

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. customthe excess thionyl chloride was removed in vacuo
  3. dissolutionThe residue was dissolved in toluene (50 mL)
  4. additionthe mixture was added to a solution of ammonia (25%, 50 mL)
  5. customA precipitate formed
  6. filtrationwas filtered off
  7. customdried