Hydrochloric Acid → HCID 135430884, compound

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Reaction Steps

To a solution of the compound obtained in Example 15 (640 mg) in pyridine (30 ml) was added acetic anhydride (336 mg) while cooling with ice. After stirring for 14 hours at room temperature, the reaction solution was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (25 ml), washed with water, dried (MgSO4), and then the solvent was distilled off. The residue was subjected to column chromatography on silica gel. The fraction eluted with hexane-ethyl acetate (5:1, v/v) was collected and the solvent was distilled off. The residue thus obtained, which was combined with saturated aqueous sodium bicarbonate (15 ml), methanol (30 ml), water (15 ml) and tetrahydrofurane (30 ml), was stirred for 3 hours at room temperature, and then neutralized with 1N hydrochloric acid. The crystal precipitated was isolated by filtration, and washed with methanol to obtain the title compound (406 mg, 58%). The product was recrystallized from tetrahydrofuran-methanol. A colorless prism crystal. M.p. 300° C. or higher.

Provenance & Evidence