반응 #68070

ord-c8877660e778476d8db4c8cbf29f30e8

용매

반응 조건

온도
57.5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    workup.STIRRINGstirred at 55-60° C. for 1 hour
  3. 3
    온도The mixture was cooled to the room temperature
  4. 4
    workup.WAITleft
  5. 5
    workup.WAITto stand for 2 nights
  6. 6
    기타The solvent was removed under reduced pressure, water
  7. 7
    workup.ADDITIONwas added
  8. 8
    workup.ADDITIONwas added
  9. 9
    기타the solvent was removed under reduced pressure
  10. 10
    workup.ADDITIONWater was added
  11. 11
    여과the resulting solid was filtered

실험 절차

To 2 mL of an ethanol solution containing 90 mg of ethyl 4-(3-(2-oxoquinoxalin-1(2H)-yl)propyl)-1-(2-(2-thienylthio)ethyl)piperidine-4-carboxylate, 0.5 mL of 20% aqueous sodium hydroxide solution was added and stirred at 55-60° C. for 5 hours. 0.5 mL of 20% aqueous sodium hydroxide solution and 0.5 mL of water were added at the same temperature, and stirred at 55-60° C. for 1 hour. The mixture was cooled to the room temperature, and left to stand for 2 nights. The solvent was removed under reduced pressure, water was added, adjusted to pH 6.5 with 6.0 mol/L hydrochloric acid, acetonitrile was added, and the solvent was removed under reduced pressure. Water was added, and the resulting solid was filtered to afford 35 mg of 4-(3-(2-oxoquinoxaline-1(2H)-yl)propyl)-1-(2-(2-thienylthio)ethyl)piperidine-4-carboxylic acid as a brown solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524738B2uspto-grants-2013_09