Sodium Carbonate → HCID 59299588, Verbindung

HRID 1097647

Reaktionsgleichung

Reaktionsgleichung von HRID 1097647
[Cl:1][C:2]1[N:10]([CH2:11][CH:12]=[CH2:13])[C:9]2[C:8](=[O:14])[NH:7][C:6](=[O:15])[NH:5][C:4]=2[N:3]=1.C(=O)([O-])[O-].[Na+].[Na+].Br[CH2:23][CH2:24][CH2:25][C:26]([F:29])([F:28])[F:27]>CN(C=O)C>[Cl:1][C:2]1[N:10]([CH2:11][CH:12]=[CH2:13])[C:9]2[C:8](=[O:14])[NH:7][C:6](=[O:15])[N:5]([CH2:23][CH2:24][CH2:25][C:26]([F:29])([F:28])[F:27])[C:4]=2[N:3]=1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 5210064-Bromo-1,1,1-trifluorobutaneHCID 592995327-Allyl-8-chloro-1H-purine-2,6(3H,7H)-dione

Produkt 1

HCID 59299588HCID 59299588, VerbindungAusbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A solution of 8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (2.0 g, 8.8 mmol) in DMF (20 ml) was treated with sodium carbonate (1.15 g, 10.8 mmol) and 4-bromo-1,1,1-trifluorobutane (1.86 g, 9.7 mmol). The mixture was stirred at 50° C. for 18 h then cooled and evaporated. The residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml). The organic phase was dried (MgSO4), filtered and evaporated. The residue was triturated in a mixture of diethyl ether and cyclohexane then the product filtered off and dried to yield the title compound as a white solid (1.18 g, 40%).

Aufarbeitung

  1. temperaturethen cooled
  2. customevaporated
  3. customThe residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml)
  4. dry with materialThe organic phase was dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was triturated in a mixture of diethyl ether and cyclohexane
  8. filtrationthe product filtered off
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9da0aabc817a471d9ca88ff34cc418da
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08143264B2

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