Réaction #311586

Équation de réaction

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

hydrazine hydrate

→

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

Solvants

ethanol

Conditions de réaction

Traitement

1. 1
   Températurewas warmed on the steam bath for 30 hours
2. 2
   TempératureThe reaction mixture was cooled
3. 3
   Autreevaporated to dryness under reduced pressure
4. 4
   AutreThe oily residue was triturated with petroleum ether (b.p. 60°-80° C.)
5. 5
   Autrethe solid product thus obtained
6. 6
   Autrewas crystallised from ethanol

Mode opératoire

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.

Source