反应 #2118732
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08686022B2
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1.9 g 1-(4-methoxy-phenyl)-2-methyl-propan-1-ol are dissolved in 30 ml dissolved, cooled to 0° C. and mixed with 3.37 ml triethylsilane. The mixture is stirred for 10 minutes and then 1.62 ml trifluoroacetic acid are added. Within 1 hour the mixture is heated to 10° C., then the reaction is stopped by the addition of water and the phases are separated. The organic phase is washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution and then dried on magnesium sulphate. The solvents are eliminated in vacuo and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 95:5 to 80:20). dissolved Within 1 hour the mixture is heated to 10° C. the phases are separated The organic phase is washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution dried on magnesium sulphate the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 95:5 to 80:20)
来源 ID: ord-2b1bef8475834188ae89eda5ffcf128e