反応 #7467

ord-455c633b370b4a5898ab60ef54ef475f

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Insoluble materials were removed by filtration
  2. 2
    その他the solvent of the filtrate was removed under reduced pressure
  3. 3
    その他The residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=1/1-1/2)

実験手順

To a solution of 4-({4-[3-(benzyloxy)propyl]phenyl}methyl)-5-trifluoromethyl-1,2-dihydro-3H-pyrazole-3-one (0.83 g) and acetobromo-α-D-glucose (1.5 g) in acetonitrile (12 mL) was added potassium carbonate (0.55 g), and the mixture was stirred at 60° C. for 20 hours. Insoluble materials were removed by filtration, and the solvent of the filtrate was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=1/1-1/2) to give 4-({4-[3-(benzyloxy)propyl]phenyl}methyl)-5-trifluoromethyl-3-(2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyloxy)-1H-pyrazole (0.64 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087579B2uspto-grants-2006_08