反应详情

温度

160 °C

A mixture of 130 mg of methanesulfonic acid 6-bromo-3-methyl-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-4-ylmethyl ester, 99 mg of 2-ethyl-2,5,5-trimethyl-piperazine-1-carboxylic acid tert-butyl ester, 0.11 ml of DIPEA and 5 mg of potassium iodide in 2 ml of dry THF was heated to 160° C. for 50 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). 75 mg (41%) 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)