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Trifluoroacetic acid → Ethyl 1-(6-amino-3,5-difluoropyridin-2-yl)-5,6,7,8-tetrafluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

HRID 1274767
ノート
印刷プレビュー

反応式

HRID 1274767 の反応式
[F:1][C:2]1[C:3]([N:19]2[C:28]3[C:23](=[C:24]([F:32])[C:25]([F:31])=[C:26]([F:30])[C:27]=3[F:29])[C:22](=[O:33])[C:21]([C:34]([O:36][CH2:37][CH3:38])=[O:35])=[CH:20]2)=[N:4][C:5]([NH:9]CC2C=CC(OC)=CC=2)=[C:6]([F:8])[CH:7]=1.FC(F)(F)C(O)=O>>[NH2:9][C:5]1[N:4]=[C:3]([N:19]2[C:28]3[C:23](=[C:24]([F:32])[C:25]([F:31])=[C:26]([F:30])[C:27]=3[F:29])[C:22](=[O:33])[C:21]([C:34]([O:36][CH2:37][CH3:38])=[O:35])=[CH:20]2)[C:2]([F:1])=[CH:7][C:6]=1[F:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 22121224Ethyl 1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridin-2-yl]-5,6,7,8-tetrafluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

生成物 1

HCID 22121241Ethyl 1-(6-amino-3,5-difluoropyridin-2-yl)-5,6,7,8-tetrafluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate収率 114.5%

実験手順

To 1080 mg of ethyl 1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridine-2-yl]-5,6,7,8-tetrafluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate was added 4 ml of trifluoroacetic acid, and the mixture was allowed to stand at room temperature for 30 minutes. The solution was concentrated under reduced pressure, and 4 ml of ethanol was added to the residue, and the solution was again concentrated under reduced pressure. The precipitate was dispersed in ethanol, collected by filtration, and washed with ethanol to obtain 960 mg of the title compound as a gray powder.

後処理

  1. concentrationThe solution was concentrated under reduced pressure, and 4 ml of ethanol
  2. additionwas added to the residue
  3. concentrationthe solution was again concentrated under reduced pressure
  4. additionThe precipitate was dispersed in ethanol
  5. filtrationcollected by filtration
  6. washwashed with ethanol

出典と根拠

ORDレコード
ord-05634b3817954397ac4bf55676532613
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06156903

反応ノート

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