Diisopropylethylamine → 2-[5-Fluoro-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-4-(3-hydroxyazetidin-1-yl)-5,5-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one

関与物質

反応条件

反応手順

100 mg (0.18 mmol, approx. 95% purity) 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 97 mg (0.89 mmol) of azetidin-3-ol hydrochloride were added. Then the reaction vessel was sealed with a septum and was heated in the microwave at 150° C. for 3 h. After cooling, water/trifluoroacetic acid was added to the reaction mixture and the resultant solid was filtered off. The filtrate was purified by preparative HPLC (acetonitrile:water (+0.1% trifluoroacetic acid) gradient). 19 mg of the title compound was obtained (21% of theor.; purity 93%).

情報源と証拠