Hydrochloric Acid → Tetrabromobisphenol A Cyanuric Chloride

Participants

Reaction Conditions

Reaction Steps

To a reaction flask equipped with a stirrer, reflux condenser, a nitrogen purge, and a temperature controlling device, were added 25.0 grams (0.136 mole) of cyanuric chloride, 331.88 grams (0.61 mole) of tetrabromobisphenol A, and a 356.88 grams of methyl ethyl ketone. While maintaining the temperature at 30° C. 34.24 grams (0.428 mole) of 50% aqueous caustic was slowly added during about 30 minutes (1800 s). The reaction mixture was stirred for an additional hour (3600 s) at 30° C., then for an additional hour (3600 s) at 60° C. The mixture was then cooled, and neutralized with hydrochloric acid, then the salt removed via water washing, then the solvent removed via vacuum distillation to about 150° C. When cooled, the product was a solid with a Mettler softening point of 126.9° C.

Provenance & Evidence