反应详情

温度

85 °C

To a solution of ethyl 4-((4-hydroxy-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxamido)(phenyl)methyl)phenyl(propyl)phosphinate, 16-f, (2.1 g, 4.16 mmol) in dioxane (30 ml) was added 2N NaOH (0.83 g, 20.8 mmol). The mixture was stirred at 85° C. for 6-8 hours, then evaporated the solvent and the residue was added water (20 ml) and extracted with ethyl acetate (30 ml) twice. The aqueous phase was adjusted to pH=1˜2 with conc. HCl, then filtered, and the filtered solid was washed with water, dried to give the title compound, 16-1, (crude product), which was further purified by prep_HPLC to give pure 16-1 (400 mg). 1H NMR (300 MHz, DMSO-d6): δ 10.38 (s, 1H), 8.61 (d, 1H), 8.42 (s, 1H), 8.06 (s, 1H), 7.34 (m, 9H), 6.72 (s, 1H), 6.32 (d, 1H), 1.75 (m, 2H), 1.41 (m, 2H), 0.95 (t, 3H). (M+H)+=478.2.

1. customevaporated the solvent
2. additionthe residue was added water (20 ml)
3. extractionextracted with ethyl acetate (30 ml) twice
4. filtrationfiltered
5. washthe filtered solid was washed with water
6. customdried