HRID1288303

反应详情

EQUATION

反应方程式

HRID 1288303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Methylsalicylamide (30.2 g; prepared as described in French Pat. No. M21) was dissolved in a solution of sodium (4.6 g.) in ethanol (200 ml.). Propyl iodide (37.4 g.) was added with stirring, and the mixture was stirred for 1 hour at room temperature and then under reflux for a further 19 hours. The mixture was concentrated to about 75 ml. and poured into water (300 ml.). The precipitated solid was filtered off and stirred with 2N sodium hydroxide solution (100 ml.). The insoluble solid was filtered off and washed with water to give crude 5-methyl-2-propoxybenzamide (37.5 g.), m.p. 112°-115° C.

WORKUP

后处理

  1. customprepared
  2. stirringthe mixture was stirred for 1 hour at room temperature
  3. temperatureunder reflux for a further 19 hours
  4. concentrationThe mixture was concentrated to about 75 ml
  5. additionand poured into water (300 ml.)
  6. filtrationThe precipitated solid was filtered off
  7. stirringstirred with 2N sodium hydroxide solution (100 ml.)
  8. filtrationThe insoluble solid was filtered off
  9. washwashed with water