반응 #2896

ord-ca2c656728094237986dc15e1b9e16c6

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITAfter a further 1 hour the mixture was allowed
  2. 2
    workup.WAITwas then left
  3. 3
    workup.STIRRINGthe mixture stirred for 5 minutes
  4. 4
    기타The organic layer was separated
  5. 5
    세척washed
  6. 6
    기타dried
  7. 7
    기타evaporated
  8. 8
    workup.DISTILLATIONThe residue was distilled

실험 절차

3-Bromofuran (20 g) was added to a solution of n-butyllithium (2.5M in hexanes, 60 ml) in diethyl ether (200 ml) at -70° C. After 30 minutes, ethyl trifluoroacetate (28.6 g) was added slowly. After a further 1 hour the mixture was allowed to warm to room temperature and was then left to stir overnight. 1M Hydrochloric acid (100 ml) was added and the mixture stirred for 5 minutes. The organic layer was separated, washed, dried and evaporated. The residue was distilled to give the title compound. B.p. 118° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05731335uspto-grants-1998_03