Dimethyl Sulfate → 2,3-Dichloro-N-methyl-N-[2-(2-oxoimidazolidin-1-yl)ethyl]benzenesulphonamide

HRID 1591754Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1591754
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9]([NH:12][CH2:13][CH2:14][N:15]1[CH2:19][CH2:18][NH:17][C:16]1=[O:20])(=[O:11])=[O:10].[C:21](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CN(C)C=O.O>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9]([N:12]([CH3:21])[CH2:13][CH2:14][N:15]1[CH2:19][CH2:18][NH:17][C:16]1=[O:20])(=[O:11])=[O:10]

Komponenten

6

Edukt 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 586387222,3-Dichloro-N-[2-(2-oxoimidazolidin-1-yl)ethyl]benzenesulphonamide

Produkt 1

HCID 586386962,3-Dichloro-N-methyl-N-[2-(2-oxoimidazolidin-1-yl)ethyl]benzenesulphonamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 0.57 g (1.69 mmol) of 2,3-dichloro-N-[2-(2-oxoimidazolidin-1-yl)ethyl]benzenesulphonamide and 0.23 g (1.7 mmol) of potassium carbonate in 10 ml dimethylformamide was stirred at room temperature for 10 minutes, 0.16 ml (1.69 mmol) of dimethyl sulphate were then added and the mixture was stirred at room temperature overnight. The mixture was then diluted with water and extracted with ethyl acetate. The combined organic extracts were dried over sodium sulphate and concentrated. The product obtained in this manner was crystallized using diethyl ether.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organic extracts were dried over sodium sulphate
  3. concentrationconcentrated
  4. customThe product obtained in this manner
  5. customwas crystallized

Quellen und Nachweise

ORD-Eintrag
ord-dd124d3ef1f74defa081155b5a2dc51a
Quelldatensatz
uspto-grants-2007_11
Patentnummer
US07291642B2

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