Methyl Methacrylate → Glycidyl methacrylate

HRID 903493

Reaktionsgleichung

Reaktionsgleichung von HRID 903493
[C:1]([O:6][CH3:7])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C-]#N.[K+].[CH2:11]1[O:13][CH:12]1CO>C1(NC2C=CC(C3C=CC(NC4C=CC=CC=4)=CC=3)=CC=2)C=CC=CC=1>[C:1]([O:6][CH2:7][CH:12]1[O:13][CH2:11]1)(=[O:5])[C:2]([CH3:4])=[CH2:3]

Komponenten

5

Edukt 3

HCID 6658Methyl MethacrylateHCID 9032Potassium CyanideHCID 11164Glycidol

Produkt 1

HCID 7837Glycidyl methacrylateAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 68280N,N'-DiphenylbenzidineKatalysator

Versuchsvorschrift

400 grams (4 moles) of methyl methacrylate, 4.74 (73 millimoles) grams of KCN and 0.118 gram (250 ppm) of N,N'-diphenylbenzidine in a 1 liter round bottom flask were heated to 90° to 100° C. with passage of air therethrough. Within one further hour there were charged 74 grams (1 mole) of glycidol and thereby the methyl methacrylate-methanol azeotrope withdrawn from the column head via a 1 meter Vigreux column at about 65° C. After 2.5 hours, the reaction was ended, which was shown by the increase of the head temperature. The sump was filtered free of potassium cyanide and washed with a little methyl methacrylate. After distilling off the methyl methacrylate there remained behind 132 grams of glycidyl methacrylate (93% yield). The product can be worked up by distillation for further purification (B.P.10, 71°-75° C.).

Aufarbeitung

  1. customthe methyl methacrylate-methanol azeotrope withdrawn from the column head via a 1 meter Vigreux column at about 65° C
  2. temperatureincrease of the head temperature
  3. filtrationThe sump was filtered free of potassium cyanide
  4. washwashed with a little methyl methacrylate
  5. distillationAfter distilling off the methyl methacrylate

Quellen und Nachweise

ORD-Eintrag
ord-36028acbb2d1470988e9d384426173e2
Quelldatensatz
uspto-grants-1980_10
Patentnummer
US04228084

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