Triethylamine → HCID 19873524, Verbindung

HRID 465276Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 465276
Cl.[CH3:2][NH:3][O:4][CH3:5].C(N(CC)CC)C.[CH3:13][NH:14][S:15](Cl)(=[O:17])=[O:16]>ClCCl>[CH3:13][NH:14][S:15]([N:3]([CH3:2])[O:4][CH3:5])(=[O:17])=[O:16]

Komponenten

5

Versuchsvorschrift

5.75 g (58.9 mmol) of N,O-dimethylhydroxylamine hydrochloride was suspended in 300 ml of dichloromethane, and 11.9 g (118 mmol) of triethylamine was added thereto. Then, the mixture was cooled with ice, and a dichloromethane solution of 7.63 g of methylsulfamoyl chloride was dropwise added, and the mixture was stirred at room temperature for 3 hours. The solvent was distilled off under reduced pressure. To the residue, 200 ml of benzene was added, and insoluble substance was filtered off. Then, the solvent was distilled off again under reduced pressure. By the distillation under reduced pressure, 4.4 g of N,N'-dimethyl-N'-methoxysulfamide was obtained (boiling point: 85°-88° C./1.9 mmHg).

Aufarbeitung

  1. temperatureThen, the mixture was cooled with ice
  2. distillationThe solvent was distilled off under reduced pressure
  3. additionTo the residue, 200 ml of benzene was added
  4. filtrationinsoluble substance was filtered off
  5. distillationThen, the solvent was distilled off again under reduced pressure
  6. distillationBy the distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-3e77ea546b56477dac491051c221d652
Quelldatensatz
uspto-grants-1992_10
Patentnummer
US05152824

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