반응 #1851982

ord-c01bd33413d94f91bfd886432926d2b3

용매

반응 조건

온도
199°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was removed under reduced pressure
  2. 2
    workup.ADDITIONTo the residue was added water (30 mL)
  3. 3
    추출extracted with CH2Cl2 (3×50 mL)
  4. 4
    세척The combined organic layers were washed with brine
  5. 5
    건조dried over MgSO4
  6. 6
    농축concentrated

실험 절차

To ethyl (6bR,10aS)-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (4.10 g, 14.3 mmol) was added n-butanol (18.0 mL) and KOH powder (3.0 g). The reaction was heated at 199° C. in a sealed tube for 18 hr. The solvent was removed under reduced pressure. To the residue was added water (30 mL) extracted with CH2Cl2 (3×50 mL). The combined organic layers were washed with brine, dried over MgSO4, and concentrated to afford the title compound as a pale yellow oil (2.70 g, 78%). MS-ESI: 216 [MH]+

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE039680E1uspto-grants-2007_06