反应详情

温度

150 °C

150 mg (0.21 mmol, purity approx. 71%) 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 dissolved, in a reaction vessel suitable for a microwave, in 1-methyl-2-pyrrolidone (3.1 ml), and 0.22 ml (1.24 mmol) of N,N-diisopropyl ethylamine and 143 mg (0.83 mmol) of tert.-butyl-azetidin-3-ylcarbamate were added. Then the reaction vessel was sealed with a septum and heated for 8 h at 150° C. in the microwave. Then 0.15 ml (0.82 mmol) of N,N-diisopropyl ethylamine and 107 mg (0.62 mmol) of tert.-butyl-azetidin-3-ylcarbamate were added again and the reaction mixture was heated for 3 h at 150° C. in the microwave. After cooling, water was added to the reaction mixture and it was purified by preparative HPLC (acetonitrile:water (+0.1% trifluoroacetic acid) gradient). 81 mg of the title compound was obtained (64% of theor.; purity 91%).

1. customThen the reaction vessel was sealed with a septum
2. temperaturethe reaction mixture was heated for 3 h at 150° C. in the microwave
3. temperatureAfter cooling
4. customwas purified by preparative HPLC (acetonitrile:water (+0.1% trifluoroacetic acid) gradient)