HRID359073

反应详情

EQUATION

反应方程式

HRID 359073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Methyl 4-hydroxy-α-methylcinnamate (16.3 g), DMF (50 ml) and anhydrous potassium carbonate (11.7 g) were mixed, and stirred at 90° C. for 1 hour. The reaction solution was allowed to cool to 50° C., added 1-bromo-3-chloropropane (8.4 ml) thereto, and the mixture was stirred at the same temperature for 1 hour. To the reaction mixture was added water (200 ml), and the mixture was extracted with ether (150 ml), washed with water (150 ml) 2 times, and then, dried over anhydrous magnesium sulfate. The ether layer was concentrated urder reduced pressure to give methyl 4-(3-chloropropoxy)-α-methylcinnamate (20 g).

WORKUP

后处理

  1. temperatureto cool to 50° C.
  2. stirringthe mixture was stirred at the same temperature for 1 hour
  3. extractionthe mixture was extracted with ether (150 ml)
  4. washwashed with water (150 ml) 2 times
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe ether layer was concentrated urder reduced pressure