반응 #68013

ord-107b4fe204144bcb9cc1d7668ea6b5b5

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITat room temperature for 5 days
  2. 2
    기타The solvent was removed under reduced pressure
  3. 3
    workup.ADDITIONthe reaction mixture was added with ethyl acetate
  4. 4
    기타The organic layer was separated
  5. 5
    추출the aqueous layer was extracted with ethyl acetate
  6. 6
    세척the resultant solution was washed with an aqueous saturated sodium chloride solution
  7. 7
    건조dried over anhydrous magnesium sulfate
  8. 8
    기타the solvent was removed under reduced pressure

실험 절차

To 0.17 g of 1-(1,3-dioxolan-2-ylmethyl)-8-methylquinolin-2(1H)-one, 2 mL of a 90% aqueous trifluoroacetic acid solution was added, and the mixture was stirred at room temperature for 4 days, at 40° C. for 3 days, and at room temperature for 5 days. The solvent was removed under reduced pressure, and the reaction mixture was added with ethyl acetate and an aqueous saturated sodium hydrogen carbonate solution. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with an aqueous saturated sodium chloride solution, and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 0.14 g of a brown oily substance, (8-methyl-2-oxoquinolin-1(2H)-yl)acetaldehyde.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524738B2uspto-grants-2013_09