反応 #350757

ord-caee3e87b39c407ca95b6b9f48757ef6

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISTILLATIONThe solvent was distilled off
  2. 2
    抽出The residue was extracted with chloroform
  3. 3
    洗浄washed
  4. 4
    その他dried
  5. 5
    その他subjected to solvent removal by distilation
  6. 6
    その他The residue was purified by silica gel column chromatography (eluent: chloroform/methanol=99/1)
  7. 7
    その他recrystallized from ethyl acetate

実験手順

In 6 ml of chloroform was dissolved 100 mg of 2-(3,4-dimethoxybenzoyl)-4-(3,4-dihydroxycarbostyril-6-yl)thiazole. Thereto was added sodium boron hydride at room temperature, and the mixture was stirred for 1 hour at the same temperature. The solvent was distilled off. The residue was extracted with chloroform. The extract was water-washed, dried and then subjected to solvent removal by distilation. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol=99/1) and then recrystallized from ethyl acetate to obtain 52 mg of 2-[1-(3,4-dimethoxyphenyl)-1-hydroxymethyl]-4-(3,4-dihydroxycarbostyril-6-yl)thiazole as light brown prismatic crystals.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05643932uspto-grants-1997_07