反应 #1701120
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08183380B2
反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 9-isopropyl-9-aza-bicyclo[3.3.1]nonan-3-one (CAS no: 56258-85-6) (5.0 g, 28 mmol) in ethanol (125 mL) and pyridine (3.3 mL, 41 mmol) with hydroxylamine hydrochloride (2.03 g, 29 mmol) was refluxed for 6 h. Cooled to 23° C., the precipitate was filtered off, washed with diethyl ether leaving a solid, which was partitioned between dichloromethane and sodium carbonate solution, the organic layers dried over Na2SO4, filtered and the solvents evaporated to give the title compound as a white solid. (4.43 g, 82%); MS: m/e=197.1 (M+H−). the precipitate was filtered off washed with diethyl ether leaving a solid, which was partitioned between dichloromethane and sodium carbonate solution the organic layers dried over Na2SO4 filtered the solvents evaporated
来源 ID: ord-405562a7eec04985a5aa1a324c7a48be