HRID978598

反应详情

EQUATION

反应方程式

HRID 978598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customTo a reaction flask equipped with a stirrer
  2. temperaturereflux condenser
  3. customa nitrogen purge
  4. addition34.24 grams (0.428 mole) of 50% aqueous caustic was slowly added during about 30 minutes (1800 s)
  5. waitfor an additional hour (3600 s) at 60° C
  6. temperatureThe mixture was then cooled
  7. customthe salt removed via water washing
  8. customthe solvent removed via vacuum distillation to about 150° C
  9. temperatureWhen cooled
  10. customwith a Mettler softening point of 126.9° C.