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Trifluoroacetic acid → HCID 66958538, Verbindung

HRID 1360422
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1360422
[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
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

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

Produkt 1

HCID 66958538HCID 66958538, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 345198Adams' catalystKatalysatorHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-df0f9c3830614a9cba2c950711fadc21
Quelldatensatz
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07879849B2

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