反应详情

A quantity of 222.45 grams (2.10 moles) of cyanogen bromide was added to a reactor containing 350 milliliters of stirred acetone under a nitrogen atmosphere. The cyanogen bromide-acetone solution was cooled to -5° C., then 228.30 grams (1.0 mole) of Bisphenol A dissolved in 700 milliliters of chilled acetone was added to the reactor. The stirred solution was allowed to equilibrate at -5° C., then 203.39 grams of triethylamine (2.01 moles) was added to the reactor over a 24-minute (1440 s) period and so as to maintain the reaction temperature at -5° C. to 0° C. After completion of the triethylamine addition, the reactor was maintained at -11° to 1° C. for 40 minutes (2400 s), followed by addition of the reaction product to 3600 milliliters of chilled water with agitation. After 5 minutes (300 s), the water and product mixture was multiply extracted with methylene chloride. The combined methylene chloride extracts were sequentially washed with dilute 5 percent hydrochloric acid, water, dilute hydrochloric acid, water and then dried over anhydrous magnesium sulfate. The dry methylene chloride extract was filtered and solvent removed by rotary evaporation under vacuum. Bisphenol A dicyanate, 265.5 grams, was recovered in 95.4 percent yield as a light tan colored crystalline solid. Infra-red spectrophotometric analysis confirmed the product structure.

1. additionwas added to the reactor
2. customto equilibrate at -5° C.
3. temperatureso as to maintain the reaction temperature at -5° C. to 0° C
4. temperaturethe reactor was maintained at -11° to 1° C. for 40 minutes (2400 s)
5. extractionthe water and product mixture was multiply extracted with methylene chloride
6. washThe combined methylene chloride extracts were sequentially washed
7. additionwith dilute 5 percent hydrochloric acid, water, dilute hydrochloric acid, water
8. dry with materialdried over anhydrous magnesium sulfate
9. extractionThe dry methylene chloride extract
10. filtrationwas filtered
11. customsolvent removed by rotary evaporation under vacuum
12. customBisphenol A dicyanate, 265.5 grams, was recovered in 95.4 percent yield as a light tan colored crystalline solid