反应详情

1.1 gm (5.0 mmols) of 7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one were suspended in 20 ml of dimethyl sulfoxide, and the suspension was mixed with 0.6 gm (5.3 mmols) of potassium tert. butylate while stirring. After 10 minutes, the solution was mixed with 2.0 gm (7.4 mmols) of 1-chloro-3-[N-methyl-N-(2-{3,4-dimethoxy-phenyl}-ethyl)-amino]-propane; the mixture was stirred for one hour at 50° C. and then poured into water; the aqueous mixture was extracted with ethyl acetate, and the organic phase was evaporated in vacuo. The residue was purified on silica gel with methylene chloride +10% of methanol as the eluant, and the dihydrochloride was precipitated from acetone with ethereal hydrochloric acid.

1. stirringthe mixture was stirred for one hour at 50° C.
2. extractionthe aqueous mixture was extracted with ethyl acetate
3. customthe organic phase was evaporated in vacuo
4. customThe residue was purified on silica gel with methylene chloride +10% of methanol as the eluant
5. customthe dihydrochloride was precipitated from acetone with ethereal hydrochloric acid