HRID260668

反应详情

EQUATION

反应方程式

HRID 260668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17.1 g (0.085 mol) of N-(7-hydroxynaphth-1-yl)acetamide in solution in 50 ml of dimethyl sulphoxide are added under a nitrogen atmosphere to a suspension of 3.4 g (0.085 mol) of sodium hydride in oil, washed beforehand with dry pentane), in 100 ml of dimethyl sulphoxide, while the mixture is cooled with an ice-water bath. Stirring is continued at room temperature for 2 h. 9.05 g (0.1 mol) of (chloromethyl)cyclopropane are added, and the mixture is stirred at room temperature for 4 h and left to stand overnight. The mixture is poured into 1 l of water, stirred for 1 h and left to stand overnight under cold conditions. The solid is separated by filtration, washed with water and dried. 13 g of a product melting point: 154°-155° C., are obtained which is used as it is in the following step.

WORKUP

后处理

  1. washwashed
  2. temperaturewhile the mixture is cooled with an ice-water bath
  3. stirringthe mixture is stirred at room temperature for 4 h
  4. waitleft
  5. waitto stand overnight
  6. stirringstirred for 1 h
  7. waitleft
  8. waitto stand overnight under cold conditions
  9. customThe solid is separated by filtration
  10. washwashed with water
  11. customdried