反应详情

温度

125 °C

A mixture of tert-butyl (1S,2R)-2-(4-(benzofuran-3-yl)-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)cyclohexylcarbamate (75 mg, 0.119 mmol) and TFA (2 mL) was placed in a vial and heated at 125° C. for 3 h. The solvent was subsequently removed in vacuo to give a residue which was dispersed in DMSO and MeOH (1/1), passed through a microfiltration frit, and purified via preparative HPLC. The fractions were collected and the solvent removed in vacuo to give a TFA salt of the title compound as a gray solid (9.2 mg, 20%). 1H NMR (500 MHz, CD3OD) δ ppm 1.67 (br s, 3H), 1.79-2.05 (m, 5H), 3.98 (br s, 1H), 4.50 (s, 2H), 4.69 (br s, 1H), 7.28-7.47 (m, 2H), 7.56 (d, J=7.81 Hz, 1H), 8.31 (d, J=6.83 Hz, 1H), 9.08 (s, 1H). [M+H] calc'd for C21H21FN4O2, 381. found, 381.

1. customThe solvent was subsequently removed in vacuo
2. customto give a residue which
3. custompurified via preparative HPLC
4. customThe fractions were collected
5. customthe solvent removed in vacuo