Dimethylformamide → 1,3-Dimethyl-6-iodoquinazolinedione

HRID 1062411

Reaktionsgleichung

Reaktionsgleichung von HRID 1062411
[H-].[Na+].[I:3][C:4]1[CH:5]=[C:6]2C(=[CH:12][CH:13]=1)N[C:9](=O)[NH:8][C:7]2=[O:15].IC.[Cl-].[NH4+].[CH3:20][N:21]([CH:23]=[O:24])[CH3:22]>>[CH3:20][N:21]1[C:22]2[C:6](=[CH:5][C:4]([I:3])=[CH:13][CH:12]=2)[C:7](=[O:15])[N:8]([CH3:9])[C:23]1=[O:24]

Komponenten

6

Edukt 5

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 113806686-iodo-1H-quinazoline-2,4-dione

Produkt 1

HCID 222873641,3-Dimethyl-6-iodoquinazolinedione

Versuchsvorschrift

Sodium hydride (0.24 g of a 60% dispersion in oil) was added portionwise to a stirred solution of 6-iodoquinazolinedione (0.58 g) (Method 53) and iodomethane (0.63 ml) in DMF (10 ml). The mixture was stirred for 1 hour then added cautiously to saturated aqueous ammonium chloride solution (200 ml). Extraction with ethyl acetate followed by recrystallization from ethanol plus a little chloroform gave the title compound (0.48 g) as a solid. MS (CI+): 317 (M+H)+.

Aufarbeitung

  1. extractionExtraction with ethyl acetate
  2. customfollowed by recrystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-d140bd268225411089a82e8db699a8d5
Quelldatensatz
uspto-grants-2005_11
Patentnummer
US06960688B2

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