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Trifluoroacetic acid → (7-methyl-2-oxoquinolin-1(2H)-yl)acetaldehyde

HRID 39687
ノート
印刷プレビュー

反応式

HRID 39687 の反応式
[O:1]1CCO[CH:2]1[CH2:6][N:7]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([CH3:17])[CH:15]=2)[CH:10]=[CH:9][C:8]1=[O:18].FC(F)(F)C(O)=O.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[CH3:17][C:14]1[CH:15]=[C:16]2[C:11]([CH:10]=[CH:9][C:8](=[O:18])[N:7]2[CH2:6][CH:2]=[O:1])=[CH:12][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 593978351-(1,3-Dioxolan-2-ylmethyl)-7-methylquinolin-2(1h)-one

生成物 1

HCID 59398276(7-methyl-2-oxoquinolin-1(2H)-yl)acetaldehyde

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To 0.37 g of 1-(1,3-dioxolan-2-ylmethyl)-7-methylquinolin-2(1H)-one, 3.7 mL of a 90% aqueous trifluoroacetic acid solution was added, the mixture was stirred at room temperature for 1 hour, and the solvent was removed under reduced pressure. The residue thus obtained was added with ethyl acetate and an aqueous saturated sodium hydrogen carbonate solution. The organic layer was separated, and the aqueous layer was extracted twice with ethyl acetate. The organic layer and an 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 0.32 g of a brown oily substance, (7-methyl-2-oxoquinolin-1(2H)-yl)acetaldehyde.

後処理

  1. customthe solvent was removed under reduced pressure
  2. customThe residue thus obtained
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted twice with ethyl acetate
  5. washthe resultant solution was washed with an aqueous saturated sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-42d0ca9f06a046c2a0dcefae39c4d806
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08524738B2

反応ノート

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