反应详情

温度

150 °C

100 mg (0.18 mmol) of 2-[5-fluoro-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 16A) was dissolved in 1-methyl-2-pyrrolidone (3.1 ml) in a reaction vessel suitable for a microwave, and 0.19 ml (1.07 mmol) of N,N-diisopropyl ethylamine and 140 mg (0.89 mmol) of 4,4-difluoropiperidine hydrochloride were added. Then the reaction vessel was sealed with a septum and was heated in the microwave for 5 h at 150° C. Then the same amounts of N,N-diisopropyl ethylamine and 4,4-difluoropiperidine hydrochloride were added again to the reaction solution and the reaction mixture was stirred for 6 h at 150° C. in the microwave. Water was added to the reaction mixture, the precipitated solid was stirred for 30 min at room temperature and then filtered off. The precipitated solid was stirred with 1 ml acetonitrile, the solid was filtered off and was washed with 0.5 ml acetonitrile. 63 mg of the target compound (64% of theor.) was obtained.

1. additionwere added
2. customThen the reaction vessel was sealed with a septum
3. stirringthe precipitated solid was stirred for 30 min at room temperature
4. filtrationfiltered off
5. stirringThe precipitated solid was stirred with 1 ml acetonitrile
6. filtrationthe solid was filtered off
7. washwas washed with 0.5 ml acetonitrile