反应详情

温度

85 °C

2,6-Dichloro-9-methyl-9H-purine (5.6 g), Na2CO3 (11.7 g), water (16.8 mL), and tetrakis(triphenylphosphine)palladium (0) (1.6 g) were added to a solution of tert-butyl 4-(2-{[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3-(trifluoromethyl)pyridin-2-yl]oxy}ethyl)piperidine-1-carboxylate (13.8 g) in dioxane (112 mL) at room temperature in an argon atmosphere, and the mixture was stirred at an internal temperature of 85° C. for 5 hours. After the reaction mixture was cooled to room temperature, water (700 mL) was added thereto, and the mixture was stirred for 3 hours. The precipitate was collected by filtration, then, washed with water and diisopropyl ether, and dried. The obtained solid was purified by silica gel column chromatography (Hex:EtOAc:CHCl3=1:1:1), whereby tert-butyl 4-(2-{[5-(2-chloro-9-methyl-9H-purin-6-yl)-3-(trifluoromethyl)pyridin-2-yl]oxy}ethyl)piperidine-1-carboxylate (9.5 g) was obtained as a solid.

1. temperatureAfter the reaction mixture was cooled to room temperature
2. stirringthe mixture was stirred for 3 hours
3. filtrationThe precipitate was collected by filtration
4. washwashed with water and diisopropyl ether
5. customdried
6. customThe obtained solid was purified by silica gel column chromatography (Hex:EtOAc:CHCl3=1:1:1)