Reaktion #83184

Reaktionsgleichung

lithium aluminum hydride

lithium aluminum hydride

alpha-butyl-alpha-phenyl-1H-1,2,4-triazole-1-propanenitrile

→

pale green oil

Ausbeute 69.2%

2-phenyl-2-[(1,2,4-triazol-1-yl)methyl]-1-hexylamine

Ausbeute 69.2%

Lösungsmittel

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigefitted with a mechanical stirrer
2. 2
   workup.STIRRINGThe reaction was stirred for an additional 5 hours after which GLC
3. 3
   SonstigeThe reaction was quenched with sodium sulfate
4. 4
   Filtrationfiltered
5. 5
   Sonstigethe organic phase separated
6. 6
   ExtraktionThe aqueous phase was extracted with 1000 mL of ether
7. 7
   Waschenwashed with 3×1.5 liters of ice water
8. 8
   Sonstigedried
9. 9
   Filtrationfiltered
10. 10
    Einengenconcentrated
11. 11
    Temperaturwithout external heating

Vorschrift

To a 5 liter flask stirring under nitrogen, fitted with a mechanical stirrer, was charged 21 g (0.55 mole) of lithium aluminum hydride. To the lithium aluminum hydride was charged 127 g (0.50 mole) alpha-butyl-alpha-phenyl-1H-1,2,4-triazole-1-propanenitrile in 2500 mL of dry ether over 2.5 hours. The reaction was stirred for an additional 5 hours after which GLC indicated the reaction was complete. The reaction was quenched with sodium sulfate, filtered and the organic phase separated. The aqueous phase was extracted with 1000 mL of ether. The organics were combined, washed with 3×1.5 liters of ice water, dried, filtered and concentrated without external heating and gave 88 g (69.2% yield) of a pale green oil.

Quelle