HRID1462624

反应详情

EQUATION

反应方程式

HRID 1462624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(4-cyanobenzyl)-3-methyl-2-(3-pyridyl)-indole (5.8 g) in 100 ml of a 1:1 mixture of 20% aqueous hydrochloric acid and glacial acetic acid was heated at reflux for 20 hours. After cooling, the solution was poured into ice water (100 ml) and the pH was adjusted to 4.5-5 with saturated sodium bicarbonate solution. The resulting precipitate was extracted with ethyl acetate, the ethyl acetate extract was washed with water and evaporated to dryness to give 1-(4-carboxybenzyl)-3-methyl-2-(3-pyridyl)indole, m.p. 273°-5°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 20 hours
  3. temperatureAfter cooling
  4. extractionThe resulting precipitate was extracted with ethyl acetate
  5. extractionthe ethyl acetate extract
  6. washwas washed with water
  7. customevaporated to dryness