Sodium Carbonate → HCID 86739859, compound

Participants

Reaction Steps

A mixture of 3.6 gm of (6.8 mmols) of 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-1,2-dion-3-yl]-3-[N-methyl-N-(2-{3,4-dimethoxy-phenyl}-ethyl)-amino]-propane, 0.57 gm of hydroxylamine hydrochloride and 0.87 gm of sodium carbonate was refluxed for 8 hours in 100 ml of ethanol. The solvent was then distilled off in vacuo; the residue was dissolved in water/methylene chloride, and the organic phase was separated, dried over magnesium sulfate and concentrated by evaporation. The residue was purified on silica gel, using methylene chloride and 5% ethanol as the eluant. The free base product thus obtained was dissolved in acetone, and the hydrochloride was precipitated by the addition of ethereal hydrochloric acid.

Provenance & Evidence