HRID2172678

反应详情

EQUATION

反应方程式

HRID 2172678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

4-Cyano-N-methylbenzamide (200 mg, 1.249 mmol), potassium carbonate (1035 mg, 7.49 mmol) and hydroxylamine hydrochloride (521 mg, 7.49 mmol) were dissolved in EtOH (12.6 mL). The reaction mixture was stirred at 80° C. for 25 h. The reaction mixture was diluted with EtOAc (50 mL), washed with water (10 mL), water phase extracted with EtOAc (20 mL). Combined organic phases were washed with brine (10 mL) and dried over sodium sulfate. The solvent was removed to yield 227 mg of a white powdery solid. The crude material was used without further purification.

WORKUP

后处理

  1. washwashed with water (10 mL), water phase
  2. extractionextracted with EtOAc (20 mL)
  3. washCombined organic phases were washed with brine (10 mL)
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed