反应详情

温度

85 °C

To a degassed mixture of 70 mg 4-[6-bromo-3-methyl-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-4-ylmethyl]-2-ethyl-2,5,5-trimethyl-piperazine-1-carboxylic acid tert-butyl ester, 21 mg 4-hydroxyphenylboronic acid and 19 mg potassium carbonate in DME/water (v/v=2/1, 0.7 mL) at r.t. and under Ar-atmosphere 2 mg palladium(0) bis(tri-tert-butylphosphine) was added and the mixture was stirred at 85° C. for 75 min in a microwave reactor. To the mixture water and ethyl acetate were added, the phases were separated and the aqueous phase was extracted with ethyl acetate. The combined organic phases were concentrated in vacuo and the resulting residue was purified by flash chromatography (silica, heptane/ethyl acetate). 19 mg (27%) of the title compound were obtained.

1. additionunder Ar-atmosphere 2 mg palladium(0) bis(tri-tert-butylphosphine) was added
2. customthe phases were separated
3. extractionthe aqueous phase was extracted with ethyl acetate
4. concentrationThe combined organic phases were concentrated in vacuo
5. customthe resulting residue was purified by flash chromatography (silica, heptane/ethyl acetate)