反应 #3217339
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05138090
反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 31.5 g (0.14 mol) of the compound from Example 3 and 9.6 ml (0.15 mol) of methyl iodide are added under a nitrogen atmosphere to 8.9 g (0.3 mol) of sodium hydride (80% strength in paraffin oil) in 500 ml of tetrahydrofuran. After stirring for 2 h at 80° C., the mixture is cautiously hydrolyzed using 30 ml of dilute hydrochloric acid, the solvent is distilled off, and the residue is taken up in methylene chloride, washed with water, dried and chromatographed on silica gel (230-400 mesh, ethyl acetate/petroleum ether 1:2). the solvent is distilled off washed with water dried chromatographed on silica gel (230-400 mesh, ethyl acetate/petroleum ether 1:2)
来源 ID: ord-8b7e1630f5c84bc9a32cc8f65f985ec8