反应详情

660 mg (2 mmol) of 3-[(hexahydro-azepin-3-yl)-methyl]-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one and 540 mg (2.2 mmol) of 2-(3,4-dimethoxyphenyl)-ethylbromide are refluxed for 1 hour in 3 ml of triethylamine. The reaction mixture is cooled and taken up in methylene chloride and 2-molar sodium hydroxide solution. The alkaline phase is separated off and extracted twice with methylene chloride. The combined organic phases are dried over magnesium sulphate and evaporated down in vacuo. Purification is carried out by column chromatography over 100 g of aluminium oxide (activity II, eluant: methylene chloride+0.3% ethanol). The fractions obtained are concentrated by evaporation in vacuo, the residue is dissolved in acetone and the hydrochloride is precipitated using ethereal hydrochloric acid.

1. temperatureThe reaction mixture is cooled
2. customThe alkaline phase is separated off
3. extractionextracted twice with methylene chloride
4. dry with materialThe combined organic phases are dried over magnesium sulphate
5. customevaporated down in vacuo
6. customPurification
7. customThe fractions obtained
8. concentrationare concentrated by evaporation in vacuo
9. dissolutionthe residue is dissolved in acetone
10. customthe hydrochloride is precipitated