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Potassium Carbonate → HCID 10430232, Verbindung

HRID 1792095
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1792095
[CH2:1]([N:3]1[C:11](=[O:12])[C:10]2[N:9]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[CH:8]=[N:7][C:6]=2[NH:5][C:4]1=[O:22])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[C:29]([O:32][CH2:33][CH2:34]Br)(=[O:31])[CH3:30]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C(#N)C>[C:29]([O:32][CH2:33][CH2:34][N:5]1[C:6]2[N:7]=[CH:8][N:9]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[C:10]=2[C:11](=[O:12])[N:3]([CH2:1][CH3:2])[C:4]1=[O:22])(=[O:31])[CH3:30]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 100657321-ethyl-3,7-dihydro-7-[(4-methoxyphenyl)methyl]-1H-Purine-2,6-dione

Produkt 1

HCID 10430232HCID 10430232, VerbindungAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 94433Tetrabutylammonium hydrogen sulfate
Katalysator
HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Acetonitrile was added to a mixture of Compound 5A (about 1.0 mole), anhydrous potassium carbonate (about 1.5 moles) and tetrabutylammonium hydrogen sulfate (about 0.05 mole). 2-bromoethyl acetate (about 1.5 moles) was added in three separate portions (0.72 mole in the beginning, another 0.45 mole after about 2 hours of reaction, and then the remaining 0.33 mole after about another 1 hour of reaction) during the course of the reaction at about 80–85° C. The total reaction time was about 7 hours. The reaction mixture was cooled to about room temperature and filtered. The filtrate was concentrated. Aqueous isopropanol was added to crystallize the product. The product was filtered, washed with aqueous isopropanol, and dried to provide Compound 6A in about a 75–80% yield.

Aufarbeitung

  1. customseparate portions (0.72 mole in the beginning
  2. customanother 0.45 mole after about 2 hours of reaction
  3. customthe remaining 0.33 mole after about another 1 hour of reaction)
  4. customduring the course of the reaction at about 80–85° C
  5. temperatureThe reaction mixture was cooled to about room temperature
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated
  8. additionAqueous isopropanol was added
  9. customto crystallize the product
  10. filtrationThe product was filtered
  11. washwashed with aqueous isopropanol
  12. customdried

Quellen und Nachweise

ORD-Eintrag
ord-417447cdb51a438bb0b0932df74ca360
Quelldatensatz
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07074923B2

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