反应详情

温度

160 °C

A mixture of 500 mg of methanesulfonic acid 6-bromo-3-methyl-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-4-ylmethyl ester, 400 mg of 2,2-diethyl-5,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester and 0.43 ml of DIPEA in 8 ml of dry THF was heated to 160° C. for 30 min in a microwave reactor. For workup the mixture was taken up in water and ethyl acetate, the phases were separated, and the aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtrated and concentrated in vacuo and the resulting residue was purified by flash chromatography (silica, heptane/ethyl acetate). 369 mg (50%) of the title compound were obtained.

1. customethyl acetate, the phases were separated
2. extractionthe aqueous phase was extracted with ethyl acetate
3. dry with materialThe combined organic phases were dried over sodium sulphate
4. filtrationfiltrated
5. concentrationconcentrated in vacuo
6. customthe resulting residue was purified by flash chromatography (silica, heptane/ethyl acetate)