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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Trifluoroacetic acid → HCID 66958538、化合物

HRID 1360422
ノート
印刷プレビュー

反応式

HRID 1360422 の反応式
[CH3:1][N:2]1[C:14]([CH2:15][CH:16]([CH3:18])[CH3:17])=[C:13]2[C:4]([C:5]([NH2:19])=[N:6][C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:12]=32)=[N:3]1.[F:20][C:21]([F:26])([F:25])[C:22]([OH:24])=[O:23]>C(Cl)(Cl)Cl.[Pt](=O)=O>[F:20][C:21]([F:26])([F:25])[C:22]([OH:24])=[O:23].[CH3:1][N:2]1[C:14]([CH2:15][CH:16]([CH3:17])[CH3:18])=[C:13]2[C:4]([C:5]([NH2:19])=[N:6][C:7]3[CH2:8][CH2:9][CH2:10][CH2:11][C:12]=32)=[N:3]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 2

HCID 6422Trifluoroacetic acidHCID 669586022-methyl-1-(2-methylpropyl)-2H-pyrazolo[3,4-c]quinolin-4-amine

生成物 1

HCID 66958538HCID 66958538、化合物

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 6212Chloroform溶媒

実験手順

A solution of 2-methyl-1-(2-methylpropyl)-2H-pyrazolo[3,4-c]quinolin-4-amine (0.6 g, 2 mmol), prepared as described in Example 3, in trifluoroacetic acid (10 mL) was treated with platinum (IV) oxide (0.5 g) and shaken under hydrogen pressure (50 psi, 3.4×105 Pa) for 24 hours. The reaction mixture was diluted with chloroform (20 mL) and filtered through a layer of CELITE filter agent. The filtrate was concentrated under reduced pressure and dissolved in chloroform (50 mL). The solution was adjusted to pH 12 with the addition of ammonium hydroxide and stirred for 20 minutes. The organic layer was separated, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The resulting solid was recrystallized from acetonitrile to provide 0.3 g of 2-methyl-1-(2-methylpropyl)-6,7,8,9-tetrahydro-2H-pyrazolo[3,4-c]quinolin-4-amine trifluoroacetate as a white powder, mp 204-206° C.

後処理

  1. filtrationfiltered through a layer of CELITE filter agent
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. dissolutiondissolved in chloroform (50 mL)
  4. additionThe solution was adjusted to pH 12 with the addition of ammonium hydroxide
  5. stirringstirred for 20 minutes
  6. customThe organic layer was separated
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe resulting solid was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-df0f9c3830614a9cba2c950711fadc21
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07879849B2

反応ノート

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