HRID2248955

反应详情

EQUATION

反应方程式

HRID 2248955 的结构方程式

PROCEDURE

实验过程

Crude 4'-acetoxyphenylmethylcarbinol (Compound II) [0.58 mol] was mixed with acetic anhydride (0.64 mol), phenothiazine (0.1 wt. %) and 85% by weight phosphoric acid (0.32 mol %). This reaction mixture was fed continuous at a rate of about 2.0 g/minute to the hot reaction vessel, as employed in Examples 1-25, and the product was collected overhead through a distillation column. The reaction vessel was immersed in hot oil maintained at 220°-230° C. and the residue temperature was maintained 180°-190° C. The product (155.4 g) containing Compound I was collected overhead through the distillation column and the residue (24.6 g) was accumulated in the hot reaction vessel. 4-Acetoxystyrene (Compound I) was isolated in 74.1% yield.

WORKUP

后处理

  1. distillationthe product was collected overhead through a distillation column
  2. temperaturemaintained at 220°-230° C.
  3. temperaturethe residue temperature was maintained 180°-190° C
  4. additionThe product (155.4 g) containing Compound I
  5. distillationwas collected overhead through the distillation column