Reaktion #582219

Reaktionsgleichung

Dihexylamine

cyanuric chloride

sodium carbonate

→

2,4-dichloro-6-dihexylamino-1,3,5-triazine

Lösungsmittel

ethyl acetate

water

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was heated
2. 2
   Temperaturto reflux for 16 h
3. 3
   Sonstigeto col to ambient temperature
4. 4
   SonstigeThe phases were separated
5. 5
   Waschenthe organic phase was washed with brine
6. 6
   Trocknendried over magnesium sulfate
7. 7
   Einengenconcentrated under reduced pressure
8. 8
   SonstigeThe crude material was purified by flash column chromatography through silica gel (elution with 3:1 hexanes:chloroform)

Vorschrift

Dihexylamine (6.3 mL, 27 mmol) was added to a mixture of cyanuric chloride (5.0 g, 27 mmol) and sodium carbonate (2.9 g, 27 mmol) in acetonitrile (50 mL). The reaction mixture was heated to reflux for 16 h and then allowed to col to ambient temperature. The mixture was diluted with ethyl acetate and water. The phases were separated and the organic phase was washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The crude material was purified by flash column chromatography through silica gel (elution with 3:1 hexanes:chloroform) to afford 2,4-dichloro-6-dihexylamino-1,3,5-triazine.

Quelle