Triethylamine → Vinylene carbonate

Participants

Reaction Steps

Monochloroethylene carbonate was prepared in the same manner as in (2) above. The prepared monochloroethylene carbonate (494 g) was dissolved in dibutyl carbonate (500 mL), and placed in a reaction vessel (2-liter volume). To the reaction vessel was dropwise added triethylamine (440 g) at 50° C. for 6 hours, for performing a reaction. The mixture was stirred further for 14 hours. The reaction mixture was cooled to room temperature, and triethylamine hydrochloride was filtered off and washed sufficiently with dibutyl carbonate. The filtrate (2,100 g) was placed at 30 mmHg to distill excessive triethylamine off, and then to collect 390 g of a vinylene carbonate distillate. The vinylene carbonate distillate was treated with silica gel and then subjected to fractional distillation at 30 mmHg to obtain 195 g of vinylene carbonate (b.p.: 73° C.) containing an extremely small amount of contaminant. The obtained vinylene carbonate was named “High purity vinylene carbonate”.

Provenance & Evidence