Propylene Glycol → 2-Methylidene-5-phenylpent-4-enoic acid

HRID 1389023

Reaktionsgleichung

Reaktionsgleichung von HRID 1389023
C(O)C(O)C.[CH2:6]=[CH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[C:14]([OH:19])(=[O:18])[C:15]([CH3:17])=[CH2:16].SC(O)C.C(OOC(C)(C)C)(=O)C>>[CH:6]([CH2:17][C:15](=[CH2:16])[C:14]([OH:19])=[O:18])=[CH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

Komponenten

6

Edukt 5

HCID 1030Propylene GlycolHCID 4093Methacrylic AcidHCID 7501StyreneHCID 61019tert-Butyl peroxyacetate2×HCID 4713212Mercapto-ethanol

Produkt 1

HCID 539699792-Methylidene-5-phenylpent-4-enoic acid

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

A 1-liter, four-necked, round bottomed flask equipped with a mechanical stirrer, two addition funnels, a distillation head with a variable takeoff, a thermometer, a nitrogen inlet, and a heating mantle atop a thermosensor-controlled pot lifter is charged with 300 g of propylene glycol. This heel charge is heated to 150° C. under nitrogen. The monomer charge (135 g styrene, 165 g methacrylic acid, and 3 g mercaptoethanol) is gradually charged over 5 hours. Simultaneously, the initiator solution (9.0 g of 70% t-butyl peracetate) is added over the same period. After completion of the feeds, an additional 0.9 g of t-butyl peracetate solution is added and the batch held at150° C. for another hour.

Aufarbeitung

  1. customA 1-liter, four-necked, round bottomed flask equipped with a mechanical stirrer
  2. additiontwo addition funnels
  3. additionThis heel charge
  4. additionis gradually charged over 5 hours
  5. waitfor another hour

Quellen und Nachweise

ORD-Eintrag
ord-0fa2c24272444f089e9852eea0bd0e34
Quelldatensatz
uspto-grants-1981_01
Patentnummer
US04243430

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