4-(3-溴苯基)丁烷-2-酮

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred mixture of pentane-2,4-dione (2.7 g, 26.7 mmol) and K2CO3 (3.4 g, 24.3 mmol) in EtOH (50 mL), 1-bromo-3-(chloromethyl)benzene (5.0 g, 24.3 mmol) was added at RT and the reaction mixture was refluxed overnight. After removal of volatiles under reduced pressure, the residue was taken up in EtOAc (100 mL) and washed with H2O (50 mL). The organic layer was separated, washed with brine, dried over Na2SO4, filtered and concentrated to afford the crude product, which was purified by silica gel column chromatography (EtOAc:Petroleum ether=1:10) to afford 4-(3-bromophenyl)butan-2-one as a colorless oil (3.7 g, 67%). MS (ES+) C10H11BrO requires: 226, 228 found: 227[M+H]+, 229 [M+2+H]+(1:1). was added at RT the reaction mixture was refluxed overnight After removal of volatiles under reduced pressure washed with H2O (50 mL) The organic layer was separated washed with brine dried over Na2SO4 filtered concentrated to afford the crude product, which was purified by silica gel column chromatography (EtOAc:Petroleum ether=1:10)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred mixture of pentane-2,4-dione (2.7 g, 26.7 mmol) and K2CO3 (3.4 g, 24.3 mmol) in EtOH (50 mL), 1-bromo-3-(chloromethyl)benzene (5.0 g, 24.3 mmol) was added at RT and the reaction mixture was refluxed overnight. After removal of volatiles under reduced pressure, the residue was taken up in EtOAc (100 mL) and washed with H2O (50 mL). The organic layer was separated, washed with brine, dried over Na2SO4, filtered and concentrated to afford the crude product, which was purified by silica gel column chromatography (EtOAc:Petroleum ether=1:10) to afford 4-(3-bromophenyl)butan-2-one as a colorless oil (3.7 g, 67%). MS (ES+) C10H11BrO requires: 226, 228 found: 227[M+H]+, 229 [M+2+H]+(1:1). was added at RT the reaction mixture was refluxed overnight After removal of volatiles under reduced pressure washed with H2O (50 mL) The organic layer was separated washed with brine dried over Na2SO4 filtered concentrated to afford the crude product, which was purified by silica gel column chromatography (EtOAc:Petroleum ether=1:10)