Hydrochloric Acid → {(8R)-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 (3.87 g, 7.32 mmol) obtained in Example 81-2) and 4 M hydrochloric acid (1,4-dioxane solution, 15 mL) in methanol (30 mL) was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure, a 5 M aqueous sodium hydroxide solution (20 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=30:70) to obtain the title compound (2.72 g, 90%) as a colorless solid.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additiona 5 M aqueous sodium hydroxide solution (20 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=30:70)

ORDレコード

ord-6e0d87dbbee14cb2b25046111c44653b

出典データセット

uspto-grants-2015_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08927536B2