反応 #350783

ord-bbd7d101004a409d857082bac060e615

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGThe mixture was stirred at room temperature for 1 hour
  2. 2
    workup.STIRRINGthe resulting mixture was stirred at the same temperature for 1 hour
  3. 3
    その他The solvent was removed from the reaction mixture by distillation
  4. 4
    workup.ADDITIONTo the residue were added
  5. 5
    その他30 ml of dichloromethane and 15 ml of water, and phase separation
  6. 6
    洗浄The organic layer was washed with 10 ml of a saturated aqueous sodium chloride solution
  7. 7
    その他dried
  8. 8
    workup.DISTILLATIONsubjected to distillation
  9. 9
    その他to remove the solvent

実験手順

In 20 ml of methanol was suspended 300 mg of 2-(3,4- diethoxyphenyl)-4-(3-methoxycarbonyl-4-hydroxy-5-formylphenyl)thiazole with stirring. Threto was added 26.5 mg of sodium boron hydride at 0° C. The mixture was stirred at room temperature for 1 hour. 26.5 mg of sodium boron hydride was further added, and the resulting mixture was stirred at the same temperature for 1 hour. The solvent was removed from the reaction mixture by distillation. To the residue were added 30 ml of dichloromethane and 15 ml of water, and phase separation was conducted. The organic layer was washed with 10 ml of a saturated aqueous sodium chloride solution, dried and subjected to distillation to remove the solvent to obtain 300 mg of 2-(3,4-diethoxyphenyl)-4-(3-methoxycarbonyl-4-hydroxy-5-hydroxymethylphenyl)-thiazole.

出典

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