Reaktion #311586

Reaktionsgleichung

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

hydrazine hydrate

→

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

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas warmed on the steam bath for 30 hours
2. 2
   TemperaturThe reaction mixture was cooled
3. 3
   Sonstigeevaporated to dryness under reduced pressure
4. 4
   SonstigeThe oily residue was triturated with petroleum ether (b.p. 60°-80° C.)
5. 5
   Sonstigethe solid product thus obtained
6. 6
   Sonstigewas crystallised from ethanol

Vorschrift

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.

Quelle