반응 #311586

반응 방정식

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

hydrazine hydrate

→

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

용매

ethanol

반응 조건

후처리

1. 1
   온도was warmed on the steam bath for 30 hours
2. 2
   온도The reaction mixture was cooled
3. 3
   기타evaporated to dryness under reduced pressure
4. 4
   기타The oily residue was triturated with petroleum ether (b.p. 60°-80° C.)
5. 5
   기타the solid product thus obtained
6. 6
   기타was crystallised from ethanol

실험 절차

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.

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