반응 #7161

ord-9e05febe729d405e925148c7270b09cc

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture is heated
  2. 2
    온도under reflux for 18 hours under argon atmosphere
  3. 3
    추출The reaction solution is extracted with ethyl acetate
  4. 4
    건조the organic layer is dried over sodium sulfate
  5. 5
    기타the solvent is evaporated under reduced pressure
  6. 6
    기타The residue is purified by silica gel column chromatography (eluent: gradient from 0% to 100% hexane/ethyl acetate)

실험 절차

Intermediate 1 (500 mg), phenylboronic acid (300 mg), tetrakis(triphenylphosphine)palladium (0) (150 mg) are dissolved in tetrahydrofuran (20 ml), and thereto are added cesium carbonate (850 mg) and water (10 ml). The mixture is heated under reflux for 18 hours under argon atmosphere. The reaction solution is extracted with ethyl acetate, and the organic layer is dried over sodium sulfate, and the solvent is evaporated under reduced pressure. The residue is purified by silica gel column chromatography (eluent: gradient from 0% to 100% hexane/ethyl acetate) to give the desired compound (360 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084176B2uspto-grants-2006_08