Acetic Acid → HCID 57061694, compound

Participants

Reaction Conditions

Reaction Steps

18.9 g of 5-chloroacenaphthene, 0.4 g of cobalt acetate tetrahydrate, 0.65 g of manganese acetate tetrahydrate, 0.2 g of NaBr, 20 ml of acetic acid, and 40 ml of benzene were charged into a reaction vessel, into which air was blown at a rate of 60 ml/min from a temperature of 65° C. The content was gradually heated up to 80° C. in 26 hours. 14 ml, in total, of acetic anhydride was dropwise added to the reaction system over the reaction time. After completion of the reaction, the solvents were removed by distillation. To residue were added 100 ml of tert-butanol and 500 ml of water dissolving 20 g of NaOH therein, to which was dropwise added 9 g of an aqueous 30% hydrogen peroxide solution at 60°-80° C. 2 hours after the dropping, the tert-butanol was removed by steam distillation. The remaining solution was treated in the same manner as in Example 8 to obtain 19.2 g of 4-chloronaphthalic anhydride in a yield of 83%.

Provenance & Evidence