反应详情

温度

150 °C

Under argon atmosphere, 150 mg (purity 62%, 0.18 mmol) of 2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-4-iodo-5,5-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one (example 15A) was suspended in 2 ml of absolute acetonitrile, and 26 mg (0.27 mmol) of 3,5-dimethyl-1H-pyrazole, 118 mg (0.36 mmol) of caesium carbonate, 5 mg (0.04 mmol) of copper(I) oxide and 20 mg (0.15 mmol) of 2-hydroxybenzaldehyde-oxime were added. The mixture was heated in the microwave for 1 h at 150° C. Then 346 mg (3.62 mmol) of 3,5-dimethyl-1H-pyrazole was added and the mixture was heated in the microwave for 45 min at 200° C. The reaction solution was filtered and purified by preparative HPLC (eluent: acetonitrile/water, gradient 20:80→100:0). 20 mg (23% of theor.) of the target compound was obtained.

1. temperaturethe mixture was heated in the microwave for 45 min at 200° C
2. filtrationThe reaction solution was filtered
3. custompurified by preparative HPLC (eluent: acetonitrile/water, gradient 20:80→100:0)
4. custom20 mg (23% of theor.) of the target compound was obtained