Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 15158208, compound

Participants

Reaction Conditions

Reaction Steps

N,O-Dimethylhydroxylamine hydrochloride (13 g, 0.12mole) was stirred in 250 mls of dichloroethane and cooled to 0° C. under argon. Triethylanime (25 g, 0.25mole) was added dropwise over 15 minutes and the mixture stirred cold for 30 minutes. The acid chloride of Example A (15 g,0.1mole) was dissolved in dichloroethane (50 mls) and added at 0° C. over 1/2 hour to the mixture. The mixture was then stirred for an additional hour at 0° C. The mixture was allowed to warm to room temperature over 2 hours and the solvent was removed in vacuo. The residue was treated with 100 mls of ethyl acetate/ether (25:75) and the triethylamine hydrochloride filtered. The filtrate was stripped of solvent and the residue distilled at 0.1 mm Hg, b.p.=62°-63° C. to give 12 g (70% yield) of the title compound.

Provenance & Evidence