HRID1288187

反应详情

EQUATION

反应方程式

HRID 1288187 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 15.0 gm (49.4 millimols) of 11-chloro-1,2,4,5-tetrahydro-3-azepino[4,5-b]quinoline-carboxylic acid ethyl ester and 28.2 gm (300 millimols) of phenol was melted at 150° C and held at that temperature for 40 hours. Then, the mixture was taken up in ethyl acetate, and the solution was extracted with dilute sodium hydroxide. The ethyl acetate phases were evaporated and chromatographed on a silicagel column with toluene/acetone (8:1) as the eluant. Subsequently, the crystals were triturated with ether/petroleum ether.

WORKUP

后处理

  1. extractionthe solution was extracted with dilute sodium hydroxide
  2. customThe ethyl acetate phases were evaporated
  3. customchromatographed on a silicagel column with toluene/acetone (8:1) as the eluant
  4. customSubsequently, the crystals were triturated with ether/petroleum ether