반응 #51725

ord-1076bffe427846ac8eb8c24fef4f4f01

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    온도to reflux overnight
  3. 3
    농축The solution was concentrated
  4. 4
    기타the residue was partitioned between H2O and CH2Cl2
  5. 5
    세척The organic phase was washed with 1N HCl and brine
  6. 6
    건조dried (MgSO4)
  7. 7
    여과filtered
  8. 8
    농축concentrated

실험 절차

2-Bromo-5-fluorobenzylbromide (2.0 g, 7.46 mmol) was dissolved in dioxane (25 mL) and H2O (25 mL), and CaCO3 (3.84 g, 38.39 mmol) was added. The mixture was heated to reflux overnight. The solution was concentrated, and the residue was partitioned between H2O and CH2Cl2. The organic phase was washed with 1N HCl and brine, dried (MgSO4), filtered, and concentrated to afford the title compound. 1H NMR (CDCl3): δ 2.00 (t, 1H), 4.72 (d, 2H), 6.85-6.92 (m, 1H), 7.26 (dd, 1H), 7.48 (dd, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06852711B2uspto-grants-2005_02