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Methyl Methacrylate → Glycidyl methacrylate

HRID 903493
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HRID 903493 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6658Methyl MethacrylateHCID 9032Potassium CyanideHCID 11164Glycidol

생성물 1

HCID 7837Glycidyl methacrylate수율 93%

시약·촉매·용매 1

HCID 68280N,N'-Diphenylbenzidine촉매

실험 절차

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further hour there were charged 74 grams (1 mole) of glycidol and thereby the methyl methacrylate-methanol azeotrope withdrawn from the column head via a 1 meter Vigreux column at about 65° C. After 2.5 hours, the reaction was ended, which was shown by the increase of the head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.).

후처리

  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 customthe methyl methacrylate-methanol azeotrope withdrawn from the column head via a 1 meter Vigreux column at about 65° C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

출처 및 근거

ORD 기록
ord-36028acbb2d1470988e9d384426173e2
출처 데이터셋
uspto-grants-1980_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04228084

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