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Diethyl Ether → N'-(2-Amino-2-methylpropyl)-N,N-dimethylsulfuric diamide

HRID 1381939
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1381939
[NH2:1][CH2:2][C:3]([NH2:6])([CH3:5])[CH3:4].CCOCC.[CH3:12][N:13]([CH3:18])[S:14](Cl)(=[O:16])=[O:15]>C(N(CC)CC)C>[CH3:4][C:3]([NH2:6])([CH3:5])[CH2:2][NH:1][S:14]([N:13]([CH3:18])[CH3:12])(=[O:16])=[O:15]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 131282-MethylpropylenediamineHCID 83372Dimethylsulphamoyl chloride

Produkt 1

HCID 13603865N'-(2-Amino-2-methylpropyl)-N,N-dimethylsulfuric diamideAusbeute 60,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A mixture of 30.7 g (0.35 mole) of 1,2-diamino-2-methylpropane, 150 ml of ether and 50 ml of triethylamine was cooled to 0° C. and 20 g (0.14 mole) of dimethylsulfamoylchloride was added slowly. The mixture was stirred for 30 min. and then concentrated under reduced pressure. The residue was mised with water, basified with potassium carbonate and concentrated to dryness. Acetone was added and insoluble material was removed by filtration. Concentration of the filtrate gave a solid, which crystallized from toluene to give 16.5 g (60%) of product, m.p. 77°-78° C. The IR and MNR spectra were consistent with the assigned structure.

Aufarbeitung

  1. concentrationconcentrated under reduced pressure
  2. concentrationconcentrated to dryness
  3. additionAcetone was added
  4. custominsoluble material was removed by filtration
  5. customConcentration of the filtrate gave a solid, which
  6. customcrystallized from toluene

Quellen und Nachweise

ORD-Eintrag
ord-4a7e1ef0a87f477085251163eaa5856a
Quelldatensatz
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04804677

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