HRID364934

反应详情

EQUATION

反应方程式

HRID 364934 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 8 hours. After cooling, the reaction mixture is diluted with water and filtered. The filtrate is acidified with 6 N hydrochloric acid and the precipitate is collected. This solid is boiled in 1 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