HRID735406

反应详情

EQUATION

反应方程式

HRID 735406 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

(2-Fluoro-3-trifluoromethyl-phenyl)-(4-methoxy-phenyl)-methanone (59.6 mg, 0.2 mmol) was dissolved in 1 ml of pyridine. Hydrazine hydrate (97 μl, 2 mmol) and 4-(dimethylamino)-pyridine (24.4 mg, 0.2 mmol) were added. The reaction mixture was stirred overnight at 100° C. After cooling to room temperature, EtOAc and 1M HCl were added. The organic phase was washed three times with brine, dried over MgSO4 and concentrated under vacuum. Purification of the crude product by flash column chromatography on silica gel (n-heptane/ethyl acetate, 85:15) afforded 56 mg of the analytically pure product.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. washThe organic phase was washed three times with brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under vacuum
  5. customPurification of the crude product by flash column chromatography on silica gel (n-heptane/ethyl acetate, 85:15)
  6. customafforded 56 mg of the analytically pure product