HRID1380849

反应详情

EQUATION

反应方程式

HRID 1380849 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

A mixture of 1,2-dihydro-5-(4-fluorophenyl)-6-methyl-2-oxo-3-pyridinecarbonitrile (5.0 grams), imidazole (25 grams), potassium carbonate (5 grams), copper (0.5 grams) and copper (I) iodide (0.5 grams) is heated just at 200° C. for 24 hours and then at 260° C. for eight hours. After cooling, the reaction mixture is diluted with water and filtered. The filtrate is acidified with 6N hydrochloric acid and the precipitate is collected. This solid is boiled in one liter of methanol and the hot mixture is filtered. The filtrate is evaporated to a volume of 200 ml and cooled to give 0.7 grams of 1,2-dihydro-5-[4-(1H- imidazol-1-yl)phenyl]-6-methyl-2-oxo-3-pyridinecarbonitrile: mp 300°-301° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationfiltered
  3. customthe precipitate is collected
  4. filtrationthe hot mixture is filtered
  5. customThe filtrate is evaporated to a volume of 200 ml
  6. temperaturecooled