반응 #157504

ord-a14879afe27149a4b83ee9b400d8ca7d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed (water, brine)
  2. 2
    건조dried over Na2SO4
  3. 3
    농축concentrated in vacuo
  4. 4
    기타The residue was purified by flash chromatography (EtOAc/hexanes)

실험 절차

To a solution of 4-hydroxy-3-(methoxy)benzaldehyde (0.760 g; 5.00 mmol) and Et3N (1.39 mL; 10.0 mmol) in anhyd CH2Cl2 (10 mL) at 0° C. was added Tf2O (0.92 mL; 5.5 mmol), dropwise over 2 min. The mixture was allowed to warm slowly to room temperature (overnight), diluted with CH2Cl2, washed (water, brine), dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash chromatography (EtOAc/hexanes), affording the title compound as a colorless oil. 1H NMR (400 MHz, CDCl3) δ 4.01 (s, 3H), 7.42 (d, J=8.2 Hz, 1H), 7.52 (dd, J=8.2, 1.8 Hz, 1H), 7.57 (d, J=1.7 Hz, 1H), 9.99 (s, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822518B2uspto-grants-2014_09