반응 #720533

ord-2f9dc58f2b2e4ca698600ebef2e1e794

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added at 16 hours and 24 hours
  2. 2
    기타Solid was removed by filtration through a short Celite column
  3. 3
    세척washing with MeOH
  4. 4
    기타Filtrate was collected
  5. 5
    기타solvent was removed in vacuo

실험 절차

A MeOH (20 ml) solution of (8aR)-2,2-difluoro-octahydro-5,5-dimethyl-N—((S)-1-phenylethyl)indolizin-7-amine hydrogen chloride and Pd(OH)2—C (20% on activated carbon, 50% wet, 0.2 g) was hydrogenated in a Parr flask under 45 psi of hydrogen. Additional Pd(OH)2—C was added (˜0.2 g) was added at 16 hours and 24 hours, and the reaction went to completion at 39 hours monitored by LC-MS. Solid was removed by filtration through a short Celite column, washing with MeOH. Filtrate was collected, solvent was removed in vacuo. Compound (8aR)-2,2-difluoro-octahydro-5,5-dimethylindolizin-7-amine hydrogen chloride was obtained as an off-white solid and was used directly in next reaction: 0.56 g; LRMS] (M+H) ink 204.99.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09321763B2uspto-grants-2016_04