Methyl Methacrylate → Butyl Methacrylate

HRID 4894

Reaktionsgleichung

Reaktionsgleichung von HRID 4894
[C:1]([O:6][CH3:7])(=[O:5])[C:2]([CH3:4])=[CH2:3].[CH:8]1[C:21]2NC3C(=CC=CC=3)SC=2C=C[CH:9]=1>C(O)CCC>[C:1]([O:6][CH2:7][CH2:9][CH2:8][CH3:21])(=[O:5])[C:2]([CH3:4])=[CH2:3]

Komponenten

4

Edukt 2

HCID 6658Methyl MethacrylateHCID 7108Phenothiazine

Produkt 1

HCID 7354Butyl Methacrylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

Two hundred six grams of a reaction mix containing a 5:1 mole ratio of methyl methacrylate, 1-butanol, 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 60% conversion of 1-butanol with a selectivity to butyl methacrylate of 99%.

Aufarbeitung

  1. additioncontaining a 5
  2. customequipped with an agitatior
  3. distillationthermocouple, and a 10-tray Oldershaw fractional distillation column
  4. additionThirty grams of the heterogeneous zirconium vinylbenzyl acetylacetonate/styrene/divinylbenzene catalyst was added
  5. temperatureThe mixture was heated
  6. temperatureto reflux at atmospheric pressure while an azeotropic mixture of methyl methacrylate and methanol
  7. customwas removed from the upper portion of the fractionating column
  8. customwas 64°-67° C.
  9. custompot was 101°-107° C

Quellen und Nachweise

ORD-Eintrag
ord-404ac2a782b04285b1b2dc05ed2a47c8
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05242877

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