Hydrochloric Acid → HCID 18008893, compound

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Reaction Steps

To a solution of the compound of Example 1 (166 mg, 480 μmol) in ethanol (5 ml) were added hydroxylamine hydrochloride (66.7 mg, 960 μmol) and successively sodium acetate (78.7 mg, 960 μmol), and the mixture was refluxed for 3 hours. After cooling, the insolubles were filtered off and solvent was distilled off. The residue obtained was submitted to silica gel column chromatography [dichloromethane-ethanol=10:1] to obtain yellowish brown powder. After dissolved this into ethanol (10 ml), 10% palladium on carbon (containing 51.1% moisture, 50.0 mg) and successively concentrated hydrochloric acid (0.5 ml) were added and the mixture was stirred for 2 hours at room temperature under hydrogen atmosphere (4 Kgf/cm2) (392 KPa). Catalyst was filtered off using celite and solvent was distilled off. Acetone was added to the residue obtained and the crystals were collected by filtration. After washed with acetone, these were air-dried, thereby obtaining 61.2 mg of title compound as colorless powder. Yield 33%.

Provenance & Evidence