Reacción #311587

Ecuación de reacción

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

ammonium chloride

sodium azide

→

4-dichloromethylene-2-trichloromethybenzo[1,3]dioxin-6-carboxylic acid

Disolventes

dimethylsulphoxide

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawas warmed on the steam bath for 16 hours
2. 2
   TemperaturaThe reaction mixture was cooled
3. 3
   workup.ADDITIONpoured onto ice
4. 4
   FiltraciónThe white product was filtered off
5. 5
   Lavadowashed with water
6. 6
   Otrodried
7. 7
   Otrocrystallised from aqueous ethanol

Procedimiento

A mixture of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylic acid (2.08 g.), ammonium chloride (0.33 g.) and sodium azide (0.36 g.) in anhydrous dimethylsulphoxide (10 ml.) was warmed on the steam bath for 16 hours. The reaction mixture was cooled, poured onto ice and kept for 16 hours. The white product was filtered off, washed with water and dried, and crystallised from aqueous ethanol to give 4-dichloromethylene-2-trichloromethybenzo[1,3]dioxin-6-carboxylic acid, m.p. 222°-223° C.

Fuente