反应 #3474231
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06906072B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Under a nitrogen atmosphere, ethyl 4-methylpentanoate (350 mg) was dissolved in tetrahydrofuran (10 mL) at −78° C., a lithium aluminum hydride/tetrahydrofuran solution (1.0 M, 1.58 mL) was added, and the mixture was stirred. While the temperature of the mixture was naturally returned to room temperature, the mixture was stirred, and after 1.5 hours, water (0.05 mL), a 2N aqueous sodium hydroxide (0.05 mL) and water (0.15 mL) were successively added thereto, and the mixture was stirred. Further, diethyl ether was added thereto, and then the resulting insoluble matters were filtered off and the filtrate was evaporated. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate system), to give the title compound as a colorless oil (257 mg, 42%: 2 steps). was naturally returned to room temperature the mixture was stirred the mixture was stirred the resulting insoluble matters were filtered off the filtrate was evaporated The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate system)
来源 ID: ord-cb47566cf49245fb83e68747abce4840