반응 #11897

ord-c0c4244a11c84b8bb0979a414d3e20be

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After reaction
  2. 2
    기타the solvents were evaporated off under reduced pressure
  3. 3
    기타the residue partitioned between EtOAc (10 mL) & 2 M HCl (3 mL)
  4. 4
    세척The organic phase was washed with H2O (2 mL), 1 M NaOH (3 mL), & brine (2 mL)
  5. 5
    건조before being dried (MgSO4)
  6. 6
    여과Filtration & solvent evaporation

실험 절차

4-(2-oxo-4-trifluoromethyl-1,2-dihydroquinolin-6-ylmethyl)benzenesulfonyl chloride (Preparation 1, 26 mg, 65 μmol) was reacted with an excess of n-BuNH2 (190 mg, 2600 μmol) by the same procedure used for Example 1. After reaction, the solvents were evaporated off under reduced pressure & the residue partitioned between EtOAc (10 mL) & 2 M HCl (3 mL). The organic phase was washed with H2O (2 mL), 1 M NaOH (3 mL), & brine (2 mL), before being dried (MgSO4). Filtration & solvent evaporation furnished the title compound (26 mg, 84%): δH ((CD3)2SO)=0.75 (t, 3H), 1.20–1.35 (m, 4H), 2.65 (m, 2H), 4.15 (s, 2H), 6.95 (s, 1H), 7.35–7.55 (m, 5H), 7.70 (d, 2H); m/z (ES+)=480.2 [M+H+MeCN]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07098340B2uspto-grants-2006_08