HRID2035907
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
- 130 °C
PROCEDURE
实验过程
Copper(I) iodide (102 mg) was added to a mixture of picolinic acid (66.1 mg), 4-(2-aminopyridin-3-yl)phenol (500 mg), tripotassium phosphate (1710 mg), 1-bromo-4-ethylbenzene (596 mg) and DMSO (8 ml). The mixture was stirred at 130° C. under nitrogen for 4 hr. Activated carbon was added and the insoluble solid was removed by filtration through silica gel/Celite pad (eluted with EtOAc). Silica-gel was added to the filtrate and the volatiles were removed in vacuo. The mixture supported on silica-gel was purified by column chromatography (NH-silica gel, eluted with EtOAc in hexane) and concentrated to give the title compound (117 mg) as an off-white solid.
WORKUP
后处理
- additionActivated carbon was added
- customthe insoluble solid was removed by filtration through silica gel/Celite pad (eluted with EtOAc)
- additionSilica-gel was added to the filtrate
- customthe volatiles were removed in vacuo
- customwas purified by column chromatography (NH-silica gel, eluted with EtOAc in hexane)
- concentrationconcentrated