Hydrochloric Acid → 1,2-Bis(methylsulfonyl)-1,2-dimethylhydrazine

HRID 249369

Reaktionsgleichung

Reaktionsgleichung von HRID 249369
Cl.Cl.[CH3:3][NH:4][NH:5][CH3:6].[CH3:7][S:8](Cl)(=[O:10])=[O:9].Cl>>[CH3:7][S:8]([N:4]([CH3:3])[N:5]([S:8]([CH3:7])(=[O:10])=[O:9])[CH3:6])(=[O:10])=[O:9]

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 93801,2-Dimethylhydrazine dihydrochlorideHCID 31297Methanesulfonyl chloride

Produkt 1

HCID 150448651,2-Bis(methylsulfonyl)-1,2-dimethylhydrazineAusbeute 32,4 %

Versuchsvorschrift

1,2-Dimethylhydrazine dihydrochloride (2.6 g, 0.02 mol) was suspended in ice-cold dry pyridine (6 ml) and the mixture was stirred for 10 minutes. Methanesulfonyl chloride (5.0 g, 0.043 mol) was added in portions to this mixture, while maintaining the temperature between 0° and 10° C. After an additional 1 hour of stirring at 0° to 5° C., the reaction mixture was left in a freezer (-10° C.) overnight. The pH of the reaction mixture was adjusted to pH 1 with cold dilute hydrochloric acid. The solid that separated was filtered and recrystallized from ethanol (Norit A) to give 1.4 g (32%) of the title compound: m.p. 168°-169° C.; anal. (C4H12N2O4S2) C,H,N; 1H NMR (CDCl3) δ 3.1 [2s, 12H, 2(CH3SO2NCH3)].

Aufarbeitung

  1. temperaturewhile maintaining the temperature between 0° and 10° C
  2. stirringAfter an additional 1 hour of stirring at 0° to 5° C.
  3. waitthe reaction mixture was left in a freezer (-10° C.) overnight
  4. customThe solid that separated
  5. filtrationwas filtered
  6. customrecrystallized from ethanol (Norit A)

Quellen und Nachweise

ORD-Eintrag
ord-73f8c8477bce4e8d9e13c39348f1a3ba
Quelldatensatz
uspto-grants-1993_05
Patentnummer
US05214068

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