反应详情

温度

140 °C

To a Smith process vial containing a suspension of 4-chloro-6-(4-nitro-phenyl)-1-(2,2,2-trifluoro-ethyl)-1H-pyrazolo[3,4-d]pyrimidine (0.68 g, 1.9 mmol) and (1R,4R)-2-oxa-5-azabicyclo[2.2.1]heptane trifluoroacetate (prepared starting from cis-1-Boc-4-hydroxy-D-prolinate, 3.1 mmol) in ethanol (14 mL) was added triethylamine (4 mL, 31 mmol). The mixture was heated in the microwave reactor for 10 minutes at 140° C. The precipitate was collected by Buchner filtration and washed successively with methanol, water, methanol, and diethyl ether. Solid was dried under house vacuum to provide (1R,4R)-5-(6-(4-nitrophenyl)-1-(2,2,2-trifluoroethyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yl)-2-oxa-5-azabicyclo[2.2.1]heptane as a pale yellow solid (0.56 g, 70%). MS (ES+): 421.1 (M+H)+

1. additionTo a Smith process vial containing
2. filtrationThe precipitate was collected by Buchner filtration
3. washwashed successively with methanol, water, methanol, and diethyl ether
4. customSolid was dried under house vacuum