Dimethylacetamide → Butylamine

HRID 218277Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 218277
C([N:4]([CH:7](C)C)[CH2:5][CH3:6])(C)C.[CH2:10]([NH:14][C:15]1[N:20]=[C:19]([NH:21][CH2:22][CH2:23][CH2:24][CH3:25])[N:18]=C(Cl)[N:16]=1)[CH2:11][CH2:12][CH3:13].[CH3:27][C:28](N(C)C)=O>>[CH2:10]([NH2:14])[CH2:11][CH2:12][CH3:13].[CH2:10]([NH:14][C:15]1[N:20]=[C:19]([NH:21][CH2:22][CH2:23][CH2:24][CH3:25])[N:18]=[C:7]([NH:4][CH2:5][CH2:6][CH2:27][CH3:28])[N:16]=1)[CH2:11][CH2:12][CH3:13]

Komponenten

5

Edukt 3

HCID 31374Dimethylacetamide2×HCID 81531DiisopropylethylamineHCID 14045984N~2~,N~4~-Dibutyl-6-chloro-1,3,5-triazine-2,4-diamine

Produkt 2

HCID 8007ButylamineHCID 108917352,4,6-tris(butylamino)-1,3,5-triazine

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of 150 millimoles of n-butylamine in 50 ml of dimethylacetamide was prepared and cooled to 0° C. To this solution was added at 0° C. a solution of 250 millimoles of diisopropylethylamine and 50 millimoles of N,N′-dibutyl-6-chloro-[1,3,5]triazine-2,4-diamine in 50 ml of dimethylacetamide, the resulting solution was heated under reflux for 4 hours, then cooled to room temperature, and the solvent was distilled off by an evaporator. The reaction mixture was then isolated and purified by silica gel column chromatography to give N,N′,N″-tributyl-[1,3,5]triazine-2,4,6-triamine as an oily substance. The result of 1H-NMR analysis is shown in FIG. 1.

Aufarbeitung

  1. temperaturethe resulting solution was heated
  2. temperatureunder reflux for 4 hours
  3. temperaturecooled to room temperature
  4. distillationthe solvent was distilled off by an evaporator
  5. customThe reaction mixture was then isolated
  6. custompurified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-957b1d14799a401799e2b8bee0f9ed98
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08198387B2

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