HRID128148

反应详情

EQUATION

反应方程式

HRID 128148 的结构方程式

CONDITIONS

反应条件

温度
118 °C

PROCEDURE

实验过程

To a 5-liter, 4-necked round-bottomed flask fitted with a condenser, addition funnel, stirrer, and thermometer were charged 1260 g (1.71 moles) above polyisopropylphenol. A 50% NaOH solution (137.3 g, 1.71 moles) was then added and the mixture heated with stirring to reflux (118° C.) and held there for 0.5 hours. The mixture was vacuum stripped at 100° (0.5 mm) to remove water, recharged with 50 g toluene, and restripped (105°, 0.2 mm) to azeotropically remove the last traces of water. The reaction was then cooled to 65° C. and 792 g (8.55 moles) epichlorohydrin was added and the reaction heated to reflux (~120° C.) for three hours. The excess epichlorohydrin was then vacuum stripped at 120° (0.05 mm) to yield ~1450 g of the crude glycidyl ether.

WORKUP

后处理

  1. customTo a 5-liter, 4-necked round-bottomed flask fitted with a condenser, addition funnel, stirrer
  2. additionthermometer were charged 1260 g (1.71 moles) above polyisopropylphenol
  3. temperaturethe mixture heated
  4. customstripped at 100°
  5. customto remove water
  6. custom(105°, 0.2 mm)
  7. customto azeotropically remove the last traces of water
  8. temperatureThe reaction was then cooled to 65° C.
  9. temperaturethe reaction heated
  10. temperatureto reflux (~120° C.) for three hours
  11. customstripped at 120°