HRID1750079
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationthe resulting precipitate was collected by filtration
- washwashed with water
- custompurified by flash chromatography on silica gel column (elution with DCM/MeOH=60:1)