反应详情

温度

90 °C

A mixture of 1.75 g of tert-butyl 3-amino-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine-1-acetate and 1.1 g of ethyl 6-(1-benzyloxycarbonyl-4-piperidyl)-2-methanesulfonyloxyhexanoate is heated at 90° C. for 24 hours. After cooling, the reaction solution is diluted with 200 ml of ethyl acetate, and the resulting solution is washed with 30 ml of 5% aqueous phosphoric acid and water, successively, and dried over anhydrous magnesium sulfate. After the solvent is distilled off under reduced pressure, the residue is separated and purified by silica gel column chromatography (hexane:ethyl acetate=2:1), whereby the first fraction yields 0.8 g of tert-butyl 3(RS)-[5-(1-benzyloxycarbonyl-4-piperidyl)-1(SR)-ethoxycarbonylpentyl]amino-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine-1-acetate as a colorless oil.

1. temperatureAfter cooling
2. washthe resulting solution is washed with 30 ml of 5% aqueous phosphoric acid and water
3. dry with materialsuccessively, and dried over anhydrous magnesium sulfate
4. distillationAfter the solvent is distilled off under reduced pressure
5. customthe residue is separated
6. custompurified by silica gel column chromatography (hexane:ethyl acetate=2:1), whereby the first fraction