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 154 mg (0.83 mmol) of tert.-butyl-pyrrolidin-3-ylcarbamate were added. Then the reaction vessel was sealed with a septum and was heated for 6 h at 150° C. in the microwave. After cooling, water was added to the reaction mixture, and trifluoroacetic acid extracted three times with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered and concentrated by evaporation. The residue was purified by preparative HPLC (acetonitrile:water (+0.1% trifluoroacetic acid) gradient). 69 mg of the title compound was obtained (59% of theor.).

1. customThen the reaction vessel was sealed with a septum
2. temperatureAfter cooling
3. extractionextracted three times with dichloromethane
4. dry with materialThe combined organic phases were dried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated by evaporation
7. customThe residue was purified by preparative HPLC (acetonitrile:water (+0.1% trifluoroacetic acid) gradient)