反应详情

Into (S)—N-(1-(3-(3-chloro-4-cyano-5-fluorophenyl)-1H-pyrazol-1-yl)propan-2-yl)-3-(1-trityl-1H-imidazol-4-yl)-1H-pyrazole-5-carboxamide (0.139 mmol, 0.095 g) was added 4 ml of a solution containing formic acid (41.8 mmol, 1.926 g), THF (20 ml) and water (1 ml). The resulting mixture was stirred first at RT after which the temperature was raised to 50° C. for 2 h. The solvent was evaporated, ACN was added and evaporated again. This was repeated once more. The crude product was purified by preparative HPLC. 0.0169 g of the title compound was obtained. 1H-NMR (400 MHz, CDCl3): δ 1.27 (d, 3H), 4.14 (dd, 1H), 4.45 (dd, 1H), 4-57-4.64 (m, 1H), 6.29 (bs), 6.63 (d, 1H), 6.90 (s, 1H), 7.32 (d, 1H), 7.51 (d, 1H), 7.52 (s, 1H), 7.63 (dd, 1H), 7.73 (d, 1H), 7.84-7.86 (m, 1H) LC-MS: [M+1]=439.0.

1. temperaturewas raised to 50° C. for 2 h
2. customThe solvent was evaporated
3. additionACN was added
4. customevaporated again
5. customThe crude product was purified by preparative HPLC