HRID904696

反应详情

EQUATION

反应方程式

HRID 904696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 6-acetyl-4-chloro-7-hydroxy-8-propyl-quinoline-2-carboxylate (6 g; 18.6474 mmole) in 33% w/w dimethylamine in methanol (50 ml) was heated at 100° C. under pressure (autoclaved) for 24 hours. The mixture was cooled, and treated with water, concentrated, and extracted with chloroform. The extract was washed with water, dried and evaporated to give a brown solid. The solid was heated in 70% sulphuric acid (150 ml) on a steambath for 6 hours. The mixture was cooled and the pH adjusted to about 7 before extraction into chloroform. The extract was dried and evaporated to give a yellow solid (1.25 g). NMR and mass spectra were consistent with the required structure.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. concentrationconcentrated
  3. extractionextracted with chloroform
  4. washThe extract was washed with water
  5. customdried
  6. customevaporated
  7. customto give a brown solid
  8. temperatureThe mixture was cooled
  9. extractionthe pH adjusted to about 7 before extraction into chloroform
  10. customThe extract was dried
  11. customevaporated