Methacrylic Acid → Oxolan-2-yl 2-methylprop-2-enoate

HRID 1460879Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1460879
[O:1]1[CH:5]=[CH:4][CH2:3][CH2:2]1.[C:6]([OH:11])(=[O:10])[C:7]([CH3:9])=[CH2:8]>C=CC1C=CN=CC=1.Cl.C1C2NC3C(=CC=CC=3)SC=2C=CC=1>[C:6]([O:11][CH:5]1[CH2:4][CH2:3][CH2:2][O:1]1)(=[O:10])[C:7]([CH3:9])=[CH2:8]

Komponenten

5

Edukt 2

HCID 4093Methacrylic AcidHCID 709342,3-Dihydrofuran

Produkt 1

HCID 154299Oxolan-2-yl 2-methylprop-2-enoateAusbeute 71,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 7108PhenothiazineKatalysatorHCID 122453074-Vinylpyridine hydrochlorideKatalysator

Versuchsvorschrift

A mixture of 4.97 g of crosslinked poly(4-vinylpyridine hydrochloride) (Fluka Chemical Corp., catalog number 82803, 6 meq/g), 192 g (207 mL, 2.74 mol) of 2,3-dihydrofuran, 118 g (116 mL, 1.36 mol) of methacrylic acid, and 1 g of phenothiazine was heated at 2° C. per minute. When the temperature reached 45° C., an exothermic reaction caused the temperature to rise to 82° C. The catalyst was removed by filtration. NMR analysis of the filtrate showed no residual methacrylic acid. After addition of sodium carbonate and calcium hydride, excess dihydrofuran was removed with a rotary evaporator, and distillation gave 151.7 g of tetrahydrofuranyl methacrylate, b.p. 43°-44° C. (0.75 mm).

Aufarbeitung

  1. temperaturewas heated at 2° C. per minute
  2. customreached 45° C.
  3. customan exothermic reaction
  4. customto rise to 82° C
  5. customThe catalyst was removed by filtration
  6. additionAfter addition of sodium carbonate and calcium hydride, excess dihydrofuran
  7. customwas removed with a rotary evaporator, and distillation

Quellen und Nachweise

ORD-Eintrag
ord-5799a108e8504b22b21f99efd34422f8
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05072029

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