HRID454034

反应详情

EQUATION

反应方程式

HRID 454034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7-benzyloxy-4-chloroquinoline (17 g, 56 mmol), (Konishi et al. WO 96/11187), in TFA (170 ml) was heated at reflux for 2 hours. The solvent was removed under vacuum and the residue was triturated with ether, filtered and washed with ether. The solid was suspended in an aqueous solution of sodium hydrogen carbonate (5.5 g, 65 mmol in 200 ml of water) and stirred at ambient temperature for 30 minutes. The solid was collected by filtration, washed with water and dried overnight under vacuum and over phosphorus pentoxide to give 4-chloro-7-hydroxyquinoline (9.85 g, 98%).

WORKUP

后处理

  1. temperatureat reflux for 2 hours
  2. customThe solvent was removed under vacuum
  3. customthe residue was triturated with ether
  4. filtrationfiltered
  5. washwashed with ether
  6. filtrationThe solid was collected by filtration
  7. washwashed with water
  8. dry with materialdried overnight under vacuum and over phosphorus pentoxide