Reaktion #311588

Reaktionsgleichung

6-cyano-2,4-bis(trichloromethyl)benzo[1,3]dioxin

ammonium chloride

sodium azide

→

4-dichloromethylene-6-(tetrazol-5-yl)-2-trichloromethylbenzo[1,3]dioxin

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas warmed on the steam bath for 16 hours
2. 2
   TemperaturThe reaction mixture was cooled
3. 3
   workup.ADDITIONpoured onto ice
4. 4
   FiltrationThe amorphous white product was filtered off
5. 5
   Sonstigetriturated with acetic acid
6. 6
   Sonstigecrystallised from chloroform

Vorschrift

A mixture of 6-cyano-2,4-bis(trichloromethyl)benzo[1,3]dioxin (1.98 g.), ammonium chloride (0.33 g.) and sodium azide in anhydrous dimethylformamide was warmed on the steam bath for 16 hours. The reaction mixture was cooled, poured onto ice and kept for 16 hours. The amorphous white product was filtered off, triturated with acetic acid, and crystallised from chloroform to give 4-dichloromethylene-6-(tetrazol-5-yl)-2-trichloromethylbenzo[1,3]dioxin, m.p. 222° C.

Quelle