反应详情

温度

70 °C

Hydrogen chloride (4 M in 1,4-dioxane) (1 mL, 0.25 mmol) was added to an ambient temperature solution of 3-[4-(2,2-dimethylpropyl)-1-trityl-1H-imidazol-2-yl]-1,1-difluoro-2-[4-(1-methyl-1H-pyrazol-5-yl)phenyl]propan-2-ol (30 mg, 0.05 mmol) in methanol (1 mL). After stirring at 70° C. for 1 h, volatiles were removed in vacuo. The residue was partitioned between diethyl ether and 1 N hydrochloric acid. The aqueous phase was washed with diethyl ether, basified with 2.5 N aqueous sodium hydroxide and extracted with ethyl acetate. Combined extracts were washed with brine, dried (sodium sulfate) and concentrated in vacuo to afford the title compound. 1H NMR (500 MHz, CD3OD) δ 7.58 (d, J=8.0 Hz, 2H), 7.46 (d, J=1.5 Hz, 1H), 7.39 (d, J=8.0 Hz, 2H), 6.51 (s, 1H), 6.30 (d, J=1.5 Hz, 1H), 5.98 (t, J=55.7 Hz, 1H), 3.81 (s, 3H), 3.42-3.28 (m, 2H), 2.31 (s, 2H), 0.76 (s, 9H).

1. customvolatiles were removed in vacuo
2. customThe residue was partitioned between diethyl ether and 1 N hydrochloric acid
3. washThe aqueous phase was washed with diethyl ether
4. extractionextracted with ethyl acetate
5. washCombined extracts were washed with brine
6. dry with materialdried (sodium sulfate)
7. concentrationconcentrated in vacuo