反应 #3435152
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08557983B2
反应条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a vigorous stirring solution of benzyl (4-oxocyclohexyl)methylcarbamate (1 g) in tetrahydrofuran (20 mL) at −78° C. was slowly added 1 M ethylmagnesium bromide (11.48 mL) in ether. After completion of the addition, the mixture was stirred at −78° C. for 2 hours and then was warmed to 0° C., and stirred in an ice bath for 30 minutes. The reaction was quenched with a cold NH4Cl aqueous solution. The precipitates were filtered off and washed with ethyl acetate. The filtrate was concentrated. The residue was dissolved in dichloromethane, loaded onto an Analogix purification system, and eluted with 0-50% ethyl acetate in dichloromethane to provide the title compound. at −78° C. After completion of the addition was warmed to 0° C. stirred in an ice bath for 30 minutes The reaction was quenched with a cold NH4Cl aqueous solution The precipitates were filtered off washed with ethyl acetate The filtrate was concentrated The residue was dissolved in dichloromethane loaded onto an Analogix purification system eluted with 0-50% ethyl acetate in dichloromethane
来源 ID: ord-f5d8a7d568624fbebd096db55111f953