Reaktion #4991

Reaktionsgleichung

methyl methacrylate

1-dodecanol

phenothiazine

→

Dodecyl Methacrylate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONcontaining a 5
2. 2
   Sonstigeequipped 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
   TemperaturThe mixture was heated
6. 6
   Temperaturto reflux at atmospheric pressure while an azeotropic mixture of methyl methacrylate and methanol
7. 7
   Sonstigewas removed from the upper portion of the fractionating column
8. 8
   Sonstigewas 64°-67° C.
9. 9
   Sonstigepot was 101°-107° C

Vorschrift

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%.

Quelle