HRID2083173

反应详情

EQUATION

反应方程式

HRID 2083173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a well stirred suspension of 45 g. of zinc dust, 90 ml. of concentrated ammonium hydroxide, 45 ml. of water and 2 ml. of cupric sulfate maintained at 80° C. there is added 14.75 g. (0.05 mole) of 3-(2-dimethylaminoethyl)-3,4-dihydro-3-phenylisocoumarin in 50 ml. ethanol for about 30 minutes. The resulting mixture is heated at 85° C. for 30 hours while a slow stream of ammonia is passed through. The mixture is filtered while under heat and the solids washed throughly with 100 ml. of hot ammonium hydroxide. The combined filtrates are cooled and carefully acidified with concentrated hydrochloric acid to give 2-(β-[-2-dimethylaminoethyl]phenethyl)benzoic acid, m.p. 152° to 154° C.

WORKUP

后处理

  1. additionsuspension of 45 g
  2. additionthere is added 14.75 g
  3. filtrationThe mixture is filtered while
  4. temperatureunder heat
  5. washthe solids washed throughly with 100 ml
  6. temperatureThe combined filtrates are cooled