반응 #92202

ord-4d6a4acf74c24c118cdab15f3f3a756d

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축concentrated to a residue which
  2. 2
    workup.ADDITIONwas diluted with EA (40 mL) and water (8 mL)
  3. 3
    건조The organic layer was dried over Na2SO4
  4. 4
    농축concentrated to a residue which
  5. 5
    기타was purified by chromatography
  6. 6
    세척eluted with PE/EA (5:1)

실험 절차

A solution of ethyl 3-(4-chlorobenzyl)-4-(3-chlorophenyl)-2-cyano-4-oxobutanoate (1.945 g, 5 mmol) in TFA (20 mL) was stirred at 100° C. for 3 h. The reaction was cooled to RT and concentrated to a residue which was diluted with EA (40 mL) and water (8 mL). The organic layer was dried over Na2SO4 and concentrated to a residue which was purified by chromatography eluted with PE/EA (5:1) to give ethyl 2-amino-4-(4-chlorobenzyl)-5-(3-chlorophenyl)furan-3-carboxylate (1.4 g, 72% yield) as a white solid. LCMS: MH+ 390 and TR=2.503 min.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447114B2uspto-grants-2016_09