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Potassium Carbonate → HCID 9801004, Verbindung

HRID 1767449
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1767449
[NH:1]1[CH2:7][CH:6]([CH2:8][OH:9])[CH2:5][NH:4][CH2:3][CH2:2]1.[CH2:10]([N:17]1[C:25]2[C:24](=[O:26])[N:23]([CH3:27])[C:22](=[O:28])[N:21]([CH3:29])[C:20]=2[N:19]=[C:18]1Cl)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:10]([N:17]1[C:25]2[C:24](=[O:26])[N:23]([CH3:27])[C:22](=[O:28])[N:21]([CH3:29])[C:20]=2[N:19]=[C:18]1[N:1]1[CH2:7][CH:6]([CH2:8][OH:9])[CH2:5][NH:4][CH2:3][CH2:2]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
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Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 3253727-Benzyl-8-chloro-1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dioneHCID 23090161(1,4-Diazepan-6-yl)methanol

Produkt 1

HCID 9801004HCID 9801004, VerbindungAusbeute 1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

([1,4]Diazepan-6-yl)methanol (1C) including potassium carbonate salts (ca 1 mmol) was suspended in dry DMF (200 ml) and 7-benzyl-8-chloro-1,3-dimethyl-3,7-dihydro-purine-2,6-dione (199.9 mg, 0.656 mmol) and potassium carbonate (453 mg, 3.28 mmol) were added. The reaction mixture was stirred at room temperature for 24 hours, heated to 60° C. for 3 hours, heated to 95° C. for 5 hours and heated to 120° C. for 2 hours. The suspension was allowed to cool to room temperature and white salts were filtered off. The filtrate was evaporated and purified by chromatography on silica, using 5% methanol in dichloromethane as the eluent. Fractions containing the product were evaporated and purified by preparative HPLC (method A2; Rt=2.52 min.) to afford 8 mg of the title compound as an yellow oil in 1% yield.

Aufarbeitung

  1. temperatureheated to 60° C. for 3 hours
  2. temperatureheated to 95° C. for 5 hours
  3. temperatureheated to 120° C. for 2 hours
  4. temperatureto cool to room temperature
  5. filtrationwhite salts were filtered off
  6. customThe filtrate was evaporated
  7. custompurified by chromatography on silica
  8. additionFractions containing the product
  9. customwere evaporated
  10. custompurified by preparative HPLC (method A2; Rt=2.52 min.)

Quellen und Nachweise

ORD-Eintrag
ord-e8729dc5a87744e685921b6c469e6d69
Quelldatensatz
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07235538B2

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