Potassium Carbonate → HCID 18366617, Verbindung

HRID 379578Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 379578
C(=O)([O-])[O-].[K+].[K+].[CH3:7][N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][S:17][C:11]=2[NH:10][C:9]1=[O:18].[CH:19]1([CH2:22]Br)[CH2:21][CH2:20]1>CN(C)C=O.O>[CH3:7][N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][S:17][C:11]=2[N:10]([CH2:22][CH:19]2[CH2:21][CH2:20]2)[C:9]1=[O:18]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 81503BromomethylcyclopropaneHCID 15085573HCID 15085573, Verbindung

Produkt 1

HCID 18366617HCID 18366617, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Potassium carbonate (1.0 g) was added to a mixture of 3-methylthieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (400 mg; J. Chem. Soc. Perkin Trans.1; 1980; 1853) and cyclopropylmethyl bromide (1.0 ml) in dry dimethylformamide (15 ml). The solution was stirred at room temperature for 20 hours and was then diluted with water and extracted thrice with diethyl ether. The combined organic extracts were washed with brine, then dried, filtered and evaporated. The residue was purified by column chromatography over silica, eluting with ethyl acetate: isohexane (1:4) to give the subtitle compound (180 mg).

Aufarbeitung

  1. extractionextracted thrice with diethyl ether
  2. washThe combined organic extracts were washed with brine
  3. customdried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by column chromatography over silica
  7. washeluting with ethyl acetate: isohexane (1:4)

Quellen und Nachweise

ORD-Eintrag
ord-ee27424c39fd47c595507e3c3bc6ca53
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06300334B1

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