HRID249970

反应详情

EQUATION

反应方程式

HRID 249970 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

4-Amino-5-cyano-2-hydroxybenzoic acid (2.1 g, 11.79 mmol) is added to a quinoline solution already heated to 160° C. (12 ml) and the reaction solution is stirred at 180° C. for a further hour. After cooling, it is diluted with about 50 ml of a 1N sodium hydroxide solution. The mixture is extracted with dichloromethane. Subsequently, the aqueous phase is adjusted to pH 6.5 with hydrochloric acid and extracted with ethyl acetate and methanol (as a solubilizer). The combined organic phases are dried over sodium sulphate. The desired product is obtained after concentrating the solvents in 76% yield (1.2 g).

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionThe mixture is extracted with dichloromethane
  3. extractionextracted with ethyl acetate and methanol (as a solubilizer)
  4. dry with materialThe combined organic phases are dried over sodium sulphate