O-methylhydroxylammonium chloride → HCID 131718641, compound

Participants

Reaction Steps

7-(2-Chloro-6-fluoro-4-trifluoromethylphenoxy)-2,4-dimethyl-2-acetyl-3,4-dihydro-3-oxo-2H-1,4-benzoxazine (Compound 93) (0.3 g) obtained in Example 15 was dissolved in pyridine (4 ml), o-methylhydroxylamine hydrochloride (0.1 g) was added, and the mixture was stirred at room temperature for 4 hours, and further, at 60° C. for one hour. The reaction mixture was then poured into ice-water, and the mixture was extracted twice with ethyl acetate (20 ml). The extract was washed with 1N-hydrochloric acid and then with saturated aqueous sodium chloride, and dried over magnesium sulfate. The solvent was evaporated under a reduced pressure, and the residue was purified by silica gel chromatography (eluant: n-hexane/ethyl acetate=4/1) to give 0.3 g of the title compound (colorless oil).

Provenance & Evidence