HRID1920838

反应详情

EQUATION

反应方程式

HRID 1920838 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 2-(2′-chloro-3′-formyl-2,4′-bipyridin-6-yl)-2-methylpropanenitrile (71 mg, 0.25 mmol) and 1M solution of hydrazine in tetrahydrofuran (3 ml) was heated under microwave irradiation at 140° C. for 20 minutes. The mixture was cooled down to room temperature, diluted with ethanol (1 ml) and hydrazine hydrate (1 ml) was added. The reaction mixture was heated under microwave irradiation at 160° C. for 30 minutes. The mixture was cooled down to room temperature, partitioned between ethyl acetate and water. The organic phase was dried over magnesium sulfate, filtered and evaporated to dryness. The residue was purified on silica gel by flash column chromatography to afford the title compound as a white solid (14.6 mg, 22% yield).

WORKUP

后处理

  1. temperatureThe mixture was cooled down to room temperature
  2. additionwas added
  3. temperatureThe reaction mixture was heated under microwave irradiation at 160° C. for 30 minutes
  4. temperatureThe mixture was cooled down to room temperature
  5. custompartitioned between ethyl acetate and water
  6. dry with materialThe organic phase was dried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated to dryness
  9. customThe residue was purified on silica gel by flash column chromatography