HRID2164265

反应详情

EQUATION

反应方程式

HRID 2164265 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(4-fluorophenyl)-2-(dimethylamino)ethenyl-2-propanone (59.6 grams), cyanoacetamide (26.7 grams) and sodium methoxide (34.3 grams) in 830 ml of dimethylformamide is heated under reflux for two hours and then the reaction mixture is concentrated on a rotary evaporator. The residual solid is suspended in water (2 liters) and is stirred overnight. The aqueous mixture is acidified with 12N HCl, diluted with water to a volume of 4 liters, and stirred for two hours. The solid product is collected, washed with water (500 ml) and then with ethanol to give 55.4 grams of 1,2-dihydro-5-(4-fluorophenyl)-6-methyl-2-oxo-3-pyridinecarbonitrile.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for two hours
  3. concentrationthe reaction mixture is concentrated on a rotary evaporator
  4. additiondiluted with water to a volume of 4 liters
  5. stirringstirred for two hours
  6. customThe solid product is collected
  7. washwashed with water (500 ml)