反应 #1618576
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08962852B2
反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Benzeneruthenium(II) chloride dimer (1.0 mg, 2 μmol, 0.5 mol %) and a chiral ligand (M=Ru, R=t-Bu, Ar=3,5-t-Bu2C6H3—, 2.6 μmol, 0.65 mol %) were dissolved in i-propanol (3 mL) under nitrogen atmosphere, and then heated and stirred for 1 h at 85° C. After the mixture was cooled to room temperature, 1-phenylbutan-1-one (0.4 mmol), i-propanol (2 mL) and a solution of sodium hydroxide in i-propanol (0.4 mL, 0.4 M) were added thereto. Thereafter, the reaction system were placed in an autoclave, and stirred for 12 h under H2 (10 atm) at 40° C. The solvent was removed under reduced pressure, and the resultants were separated by column chromatography (silica gel column; eluent:ethyl acetate/petroleum ether=1/8). Accordingly, pure 1-phenylbutynol was obtained and the ee value (ee=99.2%) was measured by GC analysis. heated After the mixture was cooled to room temperature stirred for 12 h under H2 (10 atm) at 40° C The solvent was removed under reduced pressure the resultants were separated by column chromatography (silica gel column; eluent:ethyl acetate/petroleum ether=1/8)
来源 ID: ord-dcdf5757de164be3b7b97df52b2bdb36