反応 #68013

ord-107b4fe204144bcb9cc1d7668ea6b5b5

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITat room temperature for 5 days
  2. 2
    その他The solvent was removed under reduced pressure
  3. 3
    workup.ADDITIONthe reaction mixture was added with ethyl acetate
  4. 4
    その他The organic layer was separated
  5. 5
    抽出the aqueous layer was extracted with ethyl acetate
  6. 6
    洗浄the resultant solution was washed with an aqueous saturated sodium chloride solution
  7. 7
    乾燥dried over anhydrous magnesium sulfate
  8. 8
    その他the solvent was removed under reduced pressure

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08524738B2uspto-grants-2013_09