Methacrylic Acid → Phenoxy ethylmethacrylate methylmethacrylate methacrylate

HRID 237166

Reaktionsgleichung

Reaktionsgleichung von HRID 237166
[CH2:1]([CH:3]=[C:4]([CH3:15])[C:5]([O:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:6])[CH3:2].[C:16]([OH:21])(=[O:20])[C:17]([CH3:19])=[CH2:18].[C:22]([O:27][CH3:28])(=[O:26])[C:23]([CH3:25])=[CH2:24]>C(C(C)=O)C.N(C(C)(C)C(OC)=O)=NC(C)(C)C(OC)=O>[CH2:1]([CH:3]=[C:4]([CH3:15])[C:5]([O:7][O:8][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)=[O:6])[CH3:2].[CH3:28][O:27][C:22](=[O:26])[C:23]([CH3:25])=[CH2:24].[C:16]([O-:21])(=[O:20])[C:17]([CH3:19])=[CH2:18]

Komponenten

6

Edukt 3

HCID 4093Methacrylic AcidHCID 6658Methyl MethacrylateHCID 86657890Phenoxy ethylmethacrylate

Produkt 1

HCID 86657889Phenoxy ethylmethacrylate methylmethacrylate methacrylateAusbeute 163,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 757631,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate)Katalysator2×HCID 6569Methyl Ethyl KetoneLösungsmittel3×

Reaktionsbedingungen

Temperatur
72 °C

Versuchsvorschrift

(Synthesis of Water-Insoluble Polymer Dispersant P-1) 88 g of methyl ethyl ketone was added to a 1000 ml three-necked flask equipped with an agitator and a condenser, and was heated to 72° C. under a nitrogen atmosphere. To this, a solution of 0.85 g of dimethyl 2,2′-azobisisobutyrate, 50 g of phenoxy ethylmethacrylate, 13 g of methacrylic acid and 37 g of methyl methacrylate dissolved in 50 g of methyl ethyl ketone was added dropwise over 3 hours. Once the dropwise addition was completed, the mixture was reacted for one more hour, and then a solution of 0.42 g of dimethyl 2,2′-azobisisobutyrate dissolved in 2 g of methyl ethyl ketone was added. The temperature was raised to 78° C., and the mixture was heated for 4 hours. The obtained reaction solution was precipitated two times in large excess of hexane, and the precipitated resin was dried to obtain 96.5 g of phenoxy ethylmethacrylate/methylmethacrylate/methacrylate (copolymerization ratio [% by mass ratio]=50/37/13) copolymer (resin dispersant P-1).

Aufarbeitung

  1. customequipped with an agitator and a condenser
  2. additionwas added dropwise over 3 hours
  3. additionOnce the dropwise addition
  4. customthe mixture was reacted for one more hour
  5. additionwas added
  6. temperatureThe temperature was raised to 78° C.
  7. temperaturethe mixture was heated for 4 hours
  8. customThe obtained reaction solution
  9. customwas precipitated two times in large excess of hexane
  10. customthe precipitated resin was dried

Quellen und Nachweise

ORD-Eintrag
ord-605f8938786442bf98d55b881050907d
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08641181B2

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