反应 #4991

反应方程式

methyl methacrylate

1-dodecanol

phenothiazine

→

Dodecyl Methacrylate

反应条件

后处理

1. 1
   workup.ADDITIONcontaining a 5
2. 2
   其他equipped with an agitatior
3. 3
   workup.DISTILLATIONthermocouple, and a 10-tray Oldershaw fractional distillation column
4. 4
   workup.ADDITIONThirty grams of the heterogeneous zirconium vinylbenzyl acetylacetonate/styrene/divinylbenzene catalyst was added
5. 5
   温度The mixture was heated
6. 6
   温度to reflux at atmospheric pressure while an azeotropic mixture of methyl methacrylate and methanol
7. 7
   其他was removed from the upper portion of the fractionating column
8. 8
   其他was 64°-67° C.
9. 9
   其他pot was 101°-107° C

实验过程

Two hundred six grams of a reaction mix containing a 5:1 mole ratio of methyl methacrylate, 1-dodecanol, and 100 ppm phenothiazine as inhibitor were added to a 500 ml flask equipped with an agitatior, thermocouple, and a 10-tray Oldershaw fractional distillation column. Thirty grams of the heterogeneous zirconium vinylbenzyl acetylacetonate/styrene/divinylbenzene catalyst was added. The mixture was heated to reflux at atmospheric pressure while an azeotropic mixture of methyl methacrylate and methanol was removed from the upper portion of the fractionating column. The reaction was continued in this manner for 6 hours while the temperature at the column was 64°-67° C. and the temperature in the pot was 101°-107° C. Gas liquid chromatography (GLC) analysis showed 30% conversion of 1-dodecanol with a selectivity to dodecyl methacrylate of 95%.

来源