반응 #72535

ord-3adbc94614604f3d9fa09f3bb4fa267c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at ambient temperature
  2. 2
    기타the mixture is evaporated to dryness
  3. 3
    workup.ADDITIONTo that organic phase there is added aqueous 2N HCl solution (150 ml)
  4. 4
    workup.STIRRINGthe resulting mixture is stirred
  5. 5
    기타the phases are then separated
  6. 6
    추출the aqueous phase is extracted with ethyl ether
  7. 7
    세척The organic phase is washed with saturated aqueous NaHCO3 solution and with saturated aqueous NaCl solution
  8. 8
    건조dried over sodium sulphate
  9. 9
    여과filtered
  10. 10
    기타evaporated to dryness

실험 절차

To a solution of the compound obtained in Step B (83.7 mmoles) in ethanol (200 ml) there is added, dropwise and over 20 minutes, a solution of sodium ethanolate (13.4 mmoles) in ethanol (45 ml) at ambient temperature. After stirring for 3 hours, the mixture is evaporated to dryness and then taken up in ethyl ether (200 ml). To that organic phase there is added aqueous 2N HCl solution (150 ml) and the resulting mixture is stirred; the phases are then separated and the aqueous phase is extracted with ethyl ether. The organic phase is washed with saturated aqueous NaHCO3 solution and with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness to yield the title product (brown crystals), which is used directly in the next Step.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541412B2uspto-grants-2013_09