반응 #78760

ord-d62f8cb5cdc0409eab9dad90164d7a31

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The slurry was heated
  2. 2
    온도to reflux under argon for 2 h
  3. 3
    추출extracted with ethyl acetate
  4. 4
    세척The organic layer was washed with brine
  5. 5
    건조dried (MgSO4)
  6. 6
    기타evaporated to an oil
  7. 7
    기타Purification by flash chromatography on silica gel eluting with 5% ethyl acetate in hexane

실험 절차

EX-601A) To a toluene (10 mL) solution of 3-bromofuran (0.54 mL, 6.0 mmol) was added 3-formylphenylboronic acid (1.00 g, 6.7 mmol) and DMF (4 mL). To the resulting solution was added K2CO3 (1.85 g, 13.4 mmol) and Pd(PPh3)4 (0.40 g, 0.35 mmol). The slurry was heated to reflux under argon for 2 h. The cooled mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried (MgSO4) and evaporated to an oil. Purification by flash chromatography on silica gel eluting with 5% ethyl acetate in hexane gave 0.10 g (10%) of the desired 3-(3-furanyl)benzaldehyde product as a yellow oil. MS: m/z=173.0 [M+H]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06710089B2uspto-grants-2004_03