HRID1633128

反应详情

EQUATION

反应方程式

HRID 1633128 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 is heated at reflux for 20 hours. After cooling, the solution is poured into ice water (100 ml) and the pH is adjusted to 4.5-5 with saturated sodium bicarbonate solution. The resulting precipitate is extracted with ethyl acetate, the ethyl acetate extract is washed with water and evaporated to dryness to give 1-(4-carboxybenzyl)-3-methyl-2-(3-pyridyl)indole, m.p. 273°-275°.

WORKUP

后处理

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