反应详情

温度

70 °C

Hydrogen chloride (4 M in 1,4-dioxane) (1 mL, 4 mmol) was added to an ambient temperature solution of 4-(2,2-dimethylpropyl)-2-{1-hydroxy-1-methyl-2-[4-(1-{[2-(trimethylsilyl)ethoxy]methyl}-1,4,5,6-tetrahydro-7H-pyrazolo[3,4-b]pyridin-7-yl)phenyl]ethyl}-N,N-dimethyl-1H-imidazole-1-sulfonamide (1 eq) in methanol (3 mL). After stirring at 70° C. for 1 h, volatiles were removed in vacuo. The residue was purified by high pressure liquid chromatography (KR100-5C18 100×21.2 mm column) eluting with 10-100% acetonitrile/water containing 0.05% trifluoroacetic acid. The residue was partitioned between methanol/ethyl acetate and 10% aqueous sodium hydroxide. The aqueous phase was extracted with ethyl acetate. The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo to afford the title compound. (M+H) found: 394.

1. customvolatiles were removed in vacuo
2. customThe residue was purified by high pressure liquid chromatography (KR100-5C18 100×21.2 mm column)
3. washeluting with 10-100% acetonitrile/water containing 0.05% trifluoroacetic acid
4. customThe residue was partitioned between methanol/ethyl acetate and 10% aqueous sodium hydroxide
5. extractionThe aqueous phase was extracted with ethyl acetate
6. dry with materialThe combined organic extracts were dried (magnesium sulfate)
7. concentrationconcentrated in vacuo