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Potassium Carbonate → HCID 68647620, Verbindung

HRID 1984232
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1984232
[CH3:1][C:2]([CH3:19])([CH3:18])[CH2:3][NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([OH:15])[CH:13]=2)[N:8]=[C:7]([C:16]#[N:17])[N:6]=1.Cl.[CH3:21][N:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH:23]1[CH2:28]Cl.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:1][C:2]([CH3:19])([CH3:18])[CH2:3][NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:15][CH2:28][CH:23]3[CH2:24][CH2:25][CH2:26][CH2:27][N:22]3[CH3:21])[CH:13]=2)[N:8]=[C:7]([C:16]#[N:17])[N:6]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 126443922-(Chloromethyl)-1-methylpiperidine hydrochlorideHCID 686472384-(2,2-Dimethyl-propylamino)-6-hydroxy-quinazoline-2-carbonitrile

Produkt 1

HCID 68647620HCID 68647620, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

4-(2,2-Dimethyl-propylamino)-6-hydroxy-quinazoline-2-carbonitrile (0.3 1 mmol), 1-methyl-2-chloromethyl-piperidine hydrochloride (0.41 mmol) and potassium carbonate (7.2 mmol) are stirred in DMF (3 ml) at 80° C. for 8 hours. The solvent is evaporated, the residue is dissolved in water and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and evaporated. The residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=9:1) as mobile phase. The product containing fractions are combined and evaporated. A pale oil with Rf=0.54 (CH2Cl2/MeOH=10:1) is obtained.

Aufarbeitung

  1. customThe solvent is evaporated
  2. dissolutionthe residue is dissolved in water
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customevaporated
  6. customThe residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=9:1) as mobile phase
  7. additionThe product containing fractions
  8. customevaporated
  9. customA pale oil with Rf=0.54 (CH2Cl2/MeOH=10:1) is obtained

Quellen und Nachweise

ORD-Eintrag
ord-3acbb35580ab47beb852154d94103a65
Quelldatensatz
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07544688B2

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