HRID1656438

反应详情

EQUATION

反应方程式

HRID 1656438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-amino-2'-chloro-3,5-dimethylbenzophenone (2.59 g), methyl 3,3-dimethoxypropionate (3.7 g), p-toluenesulfonic acid hydrate (0.19 g) and benzene (30 ml) was refluxed for 16 hrs., with removal of water by a Dien-Stark apparatus. The mixture was distilled to remove the solvent, and the residue was purified by a column chromatography on silica gel to give methyl 4-(2-chlorophenyl)-6,8-dimethyl-3-quinolinecarboxylate as crystals (1.90 g, 58.5%), which was recrystallized from isopropyl ether as colorless prisms. m.p. 117°-118° C.

WORKUP

后处理

  1. temperaturewas refluxed for 16 hrs
  2. custom, with removal of water by a Dien-Stark apparatus
  3. distillationThe mixture was distilled
  4. customto remove the solvent
  5. customthe residue was purified by a column chromatography on silica gel