반응 #4991

반응 방정식

methyl methacrylate

1-dodecanol

phenothiazine

→

Dodecyl Methacrylate

반응 조건

후처리

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

실험 절차

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%.

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