反应详情

温度

80 °C

A mixture of 0.52 g trans-4-[2-fluoro-2-(2-fluorophenyl)ethoxy]-cyclohexanamine hydrochloride, 0.46 g of 4-chloro-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-d]pyrimidine, and 1 g of powdered sodium carbonate in 25 mL of 2-propanol was heated to 80° C. under nitrogen overnight. The mixture was cooled, filtered and the solid washed with 3×50 mL portions of 10% methanol in chloroform. The combined extracts were concentrated under reduced pressure. Chromatography over silica gel eluting with a gradient of 50%-100% ethyl acetate in hexane gave 0.82 g of product as a white solid: MS (m+1)=458.4.

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. washthe solid washed with 3×50 mL portions of 10% methanol in chloroform
4. concentrationThe combined extracts were concentrated under reduced pressure