反应详情

温度

70 °C

Hydrogen chloride (4 M in 1,4-dioxane) (2 μL, 8 mmol) was added to an ambient temperature solution of tert-butyl [4-(4-{2-[1-[(dimethylamino)sulfonyl]-4-(2,2-dimethylpropyl)-1H-imidazo 1-2-yl]-2-hydroxypropyl}phenyl)-1-methyl-1H-pyrazol-3-yl]carbamate (33 mg, 0.06 mmol) in methanol (2 mL). After stirring at 70° C. for 1 h, volatiles were removed. The residue was purified with 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: 368.

1. customvolatiles were removed
2. customThe residue was purified with 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