Hydrochloric Acid → (3-{1-[2-Fluoro-4-(1-methyl-1H-pyrazol-4-yl)phenyl]cyclopropyl}-8-methyl-5,6,8,9-tetrahydro[1,2,4]triazolo[4,3-d][1,4]thiazepin-8-yl)methanol

A solution of the compound (368 mg, 0.70 mmol) obtained in Example 80-1) and 4 M hydrochloric acid (1,4-dioxane solution, 3 mL) in methanol (6 mL) was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure, a 5 M aqueous sodium hydroxide solution (10 mL) was added to the residue, the mixture was extracted with ethyl acetate, and the organic layer was washed with saturated sodium chloride solution and dried with anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by silica gel chromatography (ethyl acetate:methanol=20:80) to obtain the title compound (200 mg, 69%) as a colorless solid.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additiona 5 M aqueous sodium hydroxide solution (10 mL) was added to the residue
3. extractionthe mixture was extracted with ethyl acetate
4. washthe organic layer was washed with saturated sodium chloride solution
5. dry with materialdried with anhydrous sodium sulfate
6. concentrationAfter concentration under reduced pressure
7. customthe residue was purified by silica gel chromatography (ethyl acetate:methanol=20:80)

ORDレコード

ord-72d0a96a2ecf43819bf912a029feae4f

出典データセット

uspto-grants-2015_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08927536B2