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

HRID 1380594
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1380594
[NH2:1][CH2:2][C:3]([NH2:6])([CH3:5])[CH3:4].[CH3:7][N:8]([CH3:13])[S:9](Cl)(=[O:11])=[O:10]>CCOCC>[CH3:4][C:3]([NH2:6])([CH3:5])[CH2:2][NH:1][S:9]([N:8]([CH3:13])[CH3:7])(=[O:11])=[O:10]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 131282-MethylpropylenediamineHCID 83372Dimethylsulphamoyl chloride

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

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 trienthylamine 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 recrystallized 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. customrecrystallized from toluene

Quellen und Nachweise

ORD-Eintrag
ord-8f22c815e62345a28b339e85ec1a608b
Quelldatensatz
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04582855

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