反应详情

1-(4-(diphenylmethyl)piperazinyl)pentane-3-ol (940 mg) was dissolved in benzene (10 ml) and ether (10 ml), and then phosphorus tribromide (0.2 ml) was added thereto, followed by stirring the mixture overnight at room temperature. To the reaction mixture, saturated aqueous sodium hydrogen carbonate solution was added and the resultant was extracted 3 times with ethyl acetate. Organic layers were combined and washed with brine. The resultant was dried over anhydrous sodium sulfate and concentrated. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2) to obtain 340 mg of 1-(3-bromopentyl)-4-(diphenylmethyl)piperazine. Yield: 31%.

1. extractionthe resultant was extracted 3 times with ethyl acetate
2. washwashed with brine
3. dry with materialThe resultant was dried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2)