Sulfuric Acid → Hexachlorobutadiene

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

In a 1 liter flask, 200.6 g of 50% strength fuming sulphuric acid (oleum) were poured onto 300 g of 97.5% pure hexachlorocyclobutene [292.5 g (1.12 moles) of hexachlorocyclobutene; remainder hexachloro-1,3-butadiene], with stirring (molar ratio of hexachlorocyclobutene:sulphuric acid:sulphur trioxide=1:0.9:1.1). The mixture was heated at 80° C. for 5 hours. After cooling, the reaction product was poured slowly into a mixture of ice and sodium chloride, with vigorous stirring. The organic phase was then separated immediately from the aqueous phase. A mixture of 185 g of tetrachlorocyclobutenone, 14.4 g of hexachlorocyclobutene and 7.2 g of hexachloro-1,3-butadiene was obtained. The selectivity of the reaction was thus 88% of theory with a conversion of 95% of theory.

Herkunft & Nachweise