반응 #5229

ord-85ced26261244ccdada566c55d307030

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with sodium carbonate solution
  2. 2
    건조The organic layer was dried over magnesium sulfate
  3. 3
    기타the solvent was removed in vacuo
  4. 4
    기타The reaction was quenched with methanol
  5. 5
    농축The reaction mixture was concentrated in vacuo
  6. 6
    추출the resulting aqueous solution was extracted with ethyl acetate
  7. 7
    건조the organic layer was dried over magnesium sulfate
  8. 8
    기타the solvent was removed in vacuo
  9. 9
    기타The residue was triturated with ether

실험 절차

A mixture of 2-Phenyl-pyrrolo[3,4-c]quinolin-3(1H)-one (60 mg), and m-chloroperbenzoic acid (105 mg) in 3 mL of methylene chloride was kept at room temperature for 24 h. The mixture was diluted with methylene chloride and washed with sodium carbonate solution. The organic layer was dried over magnesium sulfate and the solvent was removed in vacuo. The residue was heated at 50° C. for 3 h with 1 mL of acetic anhydride. The reaction was quenched with methanol and made basic with ammonium hydroxide. The reaction mixture was concentrated in vacuo, and the resulting aqueous solution was extracted with ethyl acetate, the organic layer was dried over magnesium sulfate and the solvent was removed in vacuo. The residue was triturated with ether to afford 2-Phenyl-pyrrolo[3,4-c]quinoline-3(1H),4(5H)-dione (Compound 16) as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05243049uspto-grants-1993_09