Ethyl Methacrylate → 2-Hydroxypropyl methacrylate

HRID 634530

Reaktionsgleichung

Reaktionsgleichung von HRID 634530
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].CC1C2C(=CC3C(C=2)=CC=CC=3)C=CC=1.C(OCCCO)(=O)C(C)=C.C(OCC)(=O)C(C)=C.C([O:43][CH:44]([CH3:48])[CH2:45]OC)(=O)C>>[CH3:45][CH:44]([OH:43])[CH2:48][O:5][C:1]([C:2]([CH3:4])=[CH2:3])=[O:6]

Komponenten

5

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

A polymer feed solution was prepared by combining 30.76 g methylanthracene methacrylate monomer, 16.6 g 3-hydroxypropyl methacrylate monomer, 16.0 g ethyl methacrylate, and 50 g propylene glycol monomethyl ether acetate (PGMEA) in a 250 ml three neck, round-bottom flask fitted with a mechanical stirrer, thermal controller, thermal probe, heating mantle and nitrogen purge inlet (sweep). The reaction mixture was heated until the temperature of the reaction mixture reached 80° C. 16.15 g PGMEA solution containing 10 wt % Vazo 67 azo initiator (white powder, Dupont) was next added to the flask. The flask was heated until the temperature of the reaction mixture reached 90° C. and maintained for 8 hours with stirring. Heating was stopped and the reactor was allowed to cool down to 40° C. The resulting polymer solution was precipitated with methyl alcohol (10× excess of reaction mixture), filtered and vacuum dried, to provide Poly(ANTMA-co-HPMA-co-EMA) polymer [Mw=8K; PDI=2.5; ANTMA:HPMA; EMA=30:30:40 mol %, by 13C-NMR].

Aufarbeitung

  1. customA polymer feed solution was prepared
  2. customfitted with a mechanical stirrer
  3. temperaturethermal controller, thermal probe, heating mantle and nitrogen
  4. custompurge inlet (sweep)
  5. temperatureThe reaction mixture was heated until the temperature of the reaction mixture
  6. customreached 80° C
  7. addition16.15 g PGMEA solution containing 10 wt % Vazo 67 azo initiator (white powder, Dupont)
  8. additionwas next added to the flask
  9. temperatureThe flask was heated until the temperature of the reaction mixture
  10. customreached 90° C.
  11. temperaturemaintained for 8 hours
  12. temperatureHeating
  13. customThe resulting polymer solution was precipitated with methyl alcohol (10× excess of reaction mixture)
  14. filtrationfiltered
  15. customvacuum dried

Quellen und Nachweise

ORD-Eintrag
ord-c9da4760507f4314a70b74da3feaa588
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09324604B2

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