HRID1750079

反应详情

EQUATION

反应方程式

HRID 1750079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

AlCl3 (11.5 g, 86.3 mmol) was added portion-wise to a suspension of intermediate 13 (4.2 g, 16.6 mmol) in chlorobenzene (90 mL) at 0° C. The reaction mixture was gradually warmed to 120° C. and stirred for 3 h. The mixture was poured into ice water and the resulting precipitate was collected by filtration, washed with water, and purified by flash chromatography on silica gel column (elution with DCM/MeOH=60:1) to give 7-hydroxyquinolin-2(1H)-one (intermediate 14) (1.41 g, 53%) as a white solid.

WORKUP

后处理

  1. filtrationthe resulting precipitate was collected by filtration
  2. washwashed with water
  3. custompurified by flash chromatography on silica gel column (elution with DCM/MeOH=60:1)