Methyl iodide → HCID 14638935, Verbindung

HRID 877018Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 877018
[CH3:1][C:2]1[S:12][C:5]2[NH:6][C:7](=O)[NH:8][C:9](=[O:10])[C:4]=2[CH:3]=1.[C:13]([O-:16])([O-])=O.[K+].[K+].[CH3:19]I>CN(C=O)C.O>[CH3:19][N:6]1[C:5]2[S:12][C:2]([CH3:1])=[CH:3][C:4]=2[C:9](=[O:10])[N:8]([CH3:7])[C:13]1=[O:16]

Komponenten

6

Edukt 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 127242076-Methylthieno[2,3-d]pyrimidine-2,4(1H,3H)-dione

Produkt 1

HCID 14638935HCID 14638935, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of Step 3 intermediate (13.5 g, 74.17 mmol) in dry DMF (148 ml) was added anhydrous K2CO3 (51.25 g, 370.85 mmol) and the mixture was stirred at room temperature for 1 h. Methyl iodide (34.74 g, 244.78 mmol) was added slowly with stirring and further stirred at room temperature for 24 h. The reaction mixture was diluted with water and the solid precipitated out was filtered, washed with water and dried to give 12.6 gm of the product as a brown solid; 1H NMR (300 MHz, DMSO-d6) δ 2.42 (s, 3H), 3.22 (s, 3H), 3.42 (s, 3H), 6.90 (s, 1H).

Aufarbeitung

  1. stirringwith stirring
  2. stirringfurther stirred at room temperature for 24 h
  3. customthe solid precipitated out
  4. filtrationwas filtered
  5. washwashed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-22d7d3ce66aa47559346210f95dad6a4
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08987278B2

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