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
- 40 °C
PROCEDURE
实验过程
(R)-BINAP (1.396 g, 2.243 mmol), diacetoxypalladium (0.117 g, 0.520 mmol) and toluene (15 mL) were combined and stirred at 40° C. for 10 minutes. 7-Iodo-2-(4-methoxybenzyl)-2H-pyrazolo[4,3-b]pyridine (1.9 g, 5.20 mmol) suspended in toluene (20 mL), 2-(2,5-difluorophenyl)-5-methylpyridin-4-amine (1.146 g, 5.20 mmol) and sodium 2-methylpropan-2-olate (0.750 g, 7.80 mmol) were added and the mixture was heated at 100° C. overnight. The reaction mixture was then cooled, diluted with MeOH (10 mL) and absorbed directly onto silica and purified by column chromatography (NH silica column), eluted with EtOAc/hexanes (50-100%) to give N-(2-(2,5-difluorophenyl)-5-methylpyridin-4-yl)-1-(4-methoxybenzyl)-1H-pyrazolo[4,3-b]pyridin-7-amine and N-(2-(2,5-difluorophenyl)-5-methylpyridin-4-yl)-2-(4-methoxybenzyl)-2H-pyrazolo[4,3-b]pyridin-7-amine.
WORKUP
后处理
- temperaturethe mixture was heated at 100° C. overnight
- temperatureThe reaction mixture was then cooled
- customabsorbed directly onto silica
- custompurified by column chromatography (NH silica column)
- washeluted with EtOAc/hexanes (50-100%)