HRID1788992

反应详情

EQUATION

反应方程式

HRID 1788992 的结构方程式

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Over a 15 minute period, 149 g. (2.7 moles) of ground potassium hydroxide is added to 180 g. (0.96 mole) of 1-hydroxy-2-naphthoic acid in 2.5 l. of dimethylformamide (during the course of which the temperature rises to 32° C.). The reaction mixture is stirred at 20°-25° C. for 16 hours and at 50° C. for 2 hours and cooled to 40° C. 387 g. (2.7 moles) of methyl iodide is added, and the reaction mixture is stirred at 40°-50° C. for 4 hours. 4 l. of saturated sodium chloride solution is added, and the mixture is extracted with diethyl ether. The diethyl ether extract is dried over anhydrous sodium sulfate and evaporated at reduced pressure to obtain the crude product as a light brown oil (255 g.).

WORKUP

后处理

  1. customrises to 32° C.
  2. temperaturecooled to 40° C
  3. stirringthe reaction mixture is stirred at 40°-50° C. for 4 hours
  4. extractionthe mixture is extracted with diethyl ether
  5. extractionThe diethyl ether extract
  6. dry with materialis dried over anhydrous sodium sulfate
  7. customevaporated at reduced pressure