반응 #545932

ord-5cef6702d58541f6ae9d85b67fc2f148

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  2. 2
    workup.ADDITIONThe residue was diluted with water
  3. 3
    세척washed with diethyl ether
  4. 4
    workup.ADDITIONa saturated aqueous sodium hydrogencarbonate solution was added to the aqueous layer
  5. 5
    추출an extraction with ethyl acetate
  6. 6
    세척the organic layer was washed with saturated brine
  7. 7
    건조dried over anhydrous sodium sulfate
  8. 8
    workup.DISTILLATIONDistilling the solvent off under reduced pressure

실험 절차

162 Milligrams of t-butyl 4-((2R)-2-((1R)-3,3-difluorocyclopentyl)-2-hydroxy-2-phenylethanoyloxy)tetrahydropyridine-1(2H)-carboxylate was dissolved in 5 ml of 10% hydrochloric acid-methanol, stirred for 12 hours, and the solvent was distilled off under reduced pressure. The residue was diluted with water, washed with diethyl ether and a saturated aqueous sodium hydrogencarbonate solution was added to the aqueous layer to render it alkaline. Following an extraction with ethyl acetate, the organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. Distilling the solvent off under reduced pressure, 104 mg of the title compound was obtained as a colorless, foamy substance.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07192969B2uspto-grants-2007_03