Methyl iodide → HCID 59277705, Verbindung

HRID 1097774Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1097774
I[CH3:2].[O:3]=[S:4]1(=[O:16])[CH2:9][C:8](=O)[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[N:5]1[CH3:15].[C:17]([O-:20])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:15][N:5]1[C:6]2[CH:7]=[CH:11][CH:12]=[CH:13][C:14]=2[C:17](=[O:20])[C:9]([CH3:8])([CH3:2])[S:4]1(=[O:3])=[O:16]

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27375132,2-Dioxo-1-methyl-2,1-benzothiazin-4(3H)-one

Produkt 1

HCID 59277705HCID 59277705, VerbindungAusbeute 79,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Iodomethane (187 ul, 426 mg, 3 mmol) is added dropwise to a suspension of 2,2-Dioxo-1-methyl-2,1-benzothiazin-4(3H)-one ([CAS: 7117-31-9], 220 mg, 1 mmol), K2CO3 (1.38 g, 10 mmol) in 3 mL of dry DMF at room temperature. The resulting mixture is stirred at 60° C. After 2 h, the reaction mixture is filtered, and washed with ethyl acetate (20 mL). The combined solution is concentrated and the residue is purified by flash column (ethyl acetate-heptane v/v 10%) and gives the title compound as white solid (190 mg).

Aufarbeitung

  1. filtrationthe reaction mixture is filtered
  2. washwashed with ethyl acetate (20 mL)
  3. concentrationThe combined solution is concentrated
  4. customthe residue is purified by flash column (ethyl acetate-heptane v/v 10%)

Quellen und Nachweise

ORD-Eintrag
ord-43d21b9309a547dc84ed1ec1af739cd5
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08143278B2

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