Hydroxylamine HCl → HCID 137195736, compound

Participants

Reaction Conditions

Reaction Steps

1-[5-(tert-Butyldiphenylsilyloxymethyl)-1-(2-trimethylsilylethoxymethyl)-1H-imidazol-2-yl]ethanone (60.0 g) was dissolved in methanol (600 mL), and at room temperature hydroxylammonium chloride (16.4 g) and sodium acetate (24.2 g) were added, which mixture was subsequently warmed at 50° C., followed by stirring for 7 hours. After the reaction solution was cooled to room temperature, the insolubles were removed by filtration, and the mother liquor was concentrated to obtain the residue, which was purified by flash chromatography (ethyl acetate/hexane=10%→60%) using silica gel column (product name: Hi-Flash Column 5 L, manufactured by Yamazen Corporation) to afford the title compound (13.5 g).

Provenance & Evidence