HRID735438
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
(2-Fluoro-3-trifluoromethyl-phenyl)-(4-fluoro-phenyl)-methanone (6.58 g, 23 mmol) was dissolved in 20 ml of pyridine. Hydrazine hydrate (7.36 mL, 230 mmol) and 4-(dimethylamino)-pyridine (2.8 g, 23 mmol) were added. The reaction mixture was stirred overnight at 110° C. After cooling to room temperature, EtOAc and 2N HCl were added. The organic phase was washed three times with brine, dried over NaSO4 and concentrated under vacuum. Purification of the crude product by plug filtration (silica gel, CH2Cl2) provided 5.18 g product as a white solid.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- washThe organic phase was washed three times with brine
- dry with materialdried over NaSO4
- concentrationconcentrated under vacuum
- customPurification of the crude product
- filtrationby plug filtration (silica gel, CH2Cl2)