Dimethyl Sulfate → HCID 89620702, Verbindung

HRID 1499997Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1499997
[CH3:1][C:2]1[C:16]([S:17]([CH3:20])(=[O:19])=[O:18])=[C:15]([C:21]([F:24])([F:23])[F:22])[CH:14]=[CH:13][C:3]=1[C:4]([NH:6][C:7]1[O:8][C:9]([CH3:12])=[N:10][N:11]=1)=[O:5].[C:25]([O-])([O-])=O.[K+].[K+].S(OC)(OC)(=O)=O>CN(C=O)C>[CH3:25][N:6]([C:7]1[O:8][C:9]([CH3:12])=[N:10][N:11]=1)[C:4](=[O:5])[C:3]1[CH:13]=[CH:14][C:15]([C:21]([F:24])([F:23])[F:22])=[C:16]([S:17]([CH3:20])(=[O:19])=[O:18])[C:2]=1[CH3:1]

Komponenten

5

Edukt 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 89620381HCID 89620381, Verbindung

Produkt 1

HCID 89620702HCID 89620702, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

180 mg (0.495 mmol) of 2-methyl-N-(5-methyl-1,3,4-oxadiazol-2-yl)-3-(methylsulfonyl)-4-(trifluoromethyl)benzamide are dissolved in 6 ml of DMF (abs.), and 68 mg (0.495 mmol) of K2CO3 and 0.047 ml (0.495 mmol) of dimethyl sulfate are added. The reaction mixture is boiled under reflux for 15 hours. Then the mixture is filtered, and the filtrate is concentrated and purified by column chromatography (silica gel; heptane/ethyl acetate).

Aufarbeitung

  1. temperatureunder reflux for 15 hours
  2. filtrationThen the mixture is filtered
  3. concentrationthe filtrate is concentrated
  4. custompurified by column chromatography (silica gel; heptane/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-6c28bf76b3bf49b2b96d78a20d399b09
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09204650B2

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