HRID1186572

反应详情

EQUATION

反应方程式

HRID 1186572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-(3,5-difluoro-benzoyl)-2-fluoro-benzonitrile (2.05 g, 7.84 mmol) and hydrazine hydrate (0.73 mL, 15.7 mmol) in dry tetrahydrofuran (100 mL) was stirred at room temperature for 2 hours. The reaction mixture was treated with 37% hydrochloric acid (1.3 mL, 15.7 mmol) for 30 min and then the volatiles were partially evaporated. The reaction mixture was then diluted with water (100 mL) and aqueous NH3 was added to reach neutral pH. The resulting solid was filtered, washed thoroughly with water and dried under vacuum at 60° C. The title compound was obtained as yellow solid (1.75 g, 80% yield).

WORKUP

后处理

  1. customthe volatiles were partially evaporated
  2. additionThe reaction mixture was then diluted with water (100 mL) and aqueous NH3
  3. additionwas added
  4. filtrationThe resulting solid was filtered
  5. washwashed thoroughly with water
  6. customdried under vacuum at 60° C