Reacción #311586

Ecuación de reacción

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

hydrazine hydrate

→

4-dichloromethylene-2-trichloromethylbenzo[1,3]dioxin-6-carbohydrazide

Disolventes

ethanol

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawas warmed on the steam bath for 30 hours
2. 2
   TemperaturaThe reaction mixture was cooled
3. 3
   Otroevaporated to dryness under reduced pressure
4. 4
   OtroThe oily residue was triturated with petroleum ether (b.p. 60°-80° C.)
5. 5
   Otrothe solid product thus obtained
6. 6
   Otrowas crystallised from ethanol

Procedimiento

A mixture of ethyl 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylate (6.4 g.), 100% hydrazine hydrate (3 ml.) and ethanol (30 ml.) was warmed on the steam bath for 30 hours. The reaction mixture was cooled, and then evaporated to dryness under reduced pressure. The oily residue was triturated with petroleum ether (b.p. 60°-80° C.) and the solid product thus obtained was crystallised from ethanol, to give 4-dichloromethylene-2-trichloromethylbenzo[1,3]dioxin-6-carbohydrazide, m.p. 182°-183° C.

Fuente