反应 #1417439
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05175157
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2.9 g (0.016 mol) of 2-(2-hydroxyethyl)-hexahydro-azepinehydrochloride are liberated with concentrated sodium hydroxide solution, taken up in methylene chloride and, after drying, evaporated down over magnesium sulphate. The residue is refluxed for 2 hours with 3.9 g (0.016 mol) of 2-(3,4-dimethoxy-phenyl)ethylbromide in 10 ml of triethylamine. After cooling, the reaction mixture is combined with 2 molar sodium hydroxide solution/methylene chloride. The alkaline phase is separated off and extracted twice with methylene chloride and the combined organic phases are dried over magnesium sulphate. The solvent is distilled off in vacuo and the residue is purified by column chromatography over aluminium oxide N (activity II, eluant: methylene chloride). Yield: 3.7 g (75.2% of theory). after drying evaporated down over magnesium sulphate After cooling The alkaline phase is separated off extracted twice with methylene chloride the combined organic phases are dried over magnesium sulphate The solvent is distilled off in vacuo the residue is purified by column chromatography over aluminium oxide N (activity II, eluant: methylene chloride)
来源 ID: ord-13b7bceefe234f38b67554e0e4c2e1c6