Reaktion #8645

Reaktionsgleichung

p-t-butylbenzonitrile

lithium chloride

sodium azide

triethylammonium bromide

hydrochloric acid

→

colorless crystals

Ausbeute 70.7%

5-(4-t-butylphenyl)tetrazole

Ausbeute 70.7%

Lösungsmittel

DMF

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeIn a 250 ml round-bottomed flask fitted
2. 2
   Temperaturwith reflux condenser
3. 3
   Sonstigeprecipitates
4. 4
   FiltrationThe precipitate is filtered off with suction
5. 5
   Waschenwashed with water
6. 6
   Sonstigedried
7. 7
   SonstigeRecrystallization from ethanol/water

Vorschrift

In a 250 ml round-bottomed flask fitted with reflux condenser, 4.9 g of p-t-butylbenzonitrile, 3.82 g of lithium chloride and 5.85 g of sodium azide and 8.2 g of triethylammonium bromide in 100 ml of DMF are heated at 120° C. for 8 hours. After cooling to room temperature, 100 ml of water are added and the mixture is admicxed in an ice bath with dilute hydrochloric acid until no further solid precipitates. The precipitate is filtered off with suction, washed with water and dried. Recrystallization from ethanol/water gives 4.4 g of colorless crystals.

Quelle