反応 #161002

ord-f4f0f6771a404cb6836a508e35547aa9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture was heated
  2. 2
    温度under reflux for 3 hours
  3. 3
    洗浄to wash it
  4. 4
    抽出the mixture was extracted with ethyl acetate
  5. 5
    洗浄After the obtained organic layer was washed with saturated brine, it
  6. 6
    乾燥was dried with anhydrous sodium sulfate
  7. 7
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

実験手順

450 ml of 2N aqueous sodium hydroxide solution was added to a solution of 75.4 g (300 mmol) of 1-[(3-furanylcarbonyl)amino]cyclohexanecarboxylic acid methyl ester in 450 ml of tetrahydrofuran, and the mixture was heated under reflux for 3 hours. After ether was added to the reaction solution to wash it, the aqueous layer was neutralized by concentrated hydrochloric acid, and the mixture was extracted with ethyl acetate. After the obtained organic layer was washed with saturated brine, it was dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 68.8 g (97%) of the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08829209B2uspto-grants-2014_09