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

HRID 2107570
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2107570
[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 mol) 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 mol) of dimethylsulfamoyl chloride was added slowly. The reaction mixture was stirred for 30 minutes and evaporated to dryness. The residue was mixed with water, basified with K2CO3 and evaporated to dryness. Acetone was added and the mixture was filtered. Evaporation of the filtrate gave a solid which was recrystalized from toluene to give 16.5 g (60.3%) of product, mp 77°-78° C. The NMR and IR were consistent with the assigned structure.

Aufarbeitung

  1. customevaporated to dryness
  2. additionThe residue was mixed with water
  3. customevaporated to dryness
  4. additionAcetone was added
  5. filtrationthe mixture was filtered
  6. customEvaporation of the filtrate
  7. customgave a solid which
  8. customwas recrystalized from toluene

Quellen und Nachweise

ORD-Eintrag
ord-de74ef9d955d4bdda0d924e05b050262
Quelldatensatz
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04935421

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