Methanol → NaMAU AMPS

HRID 405652

Reaktionsgleichung

Reaktionsgleichung von HRID 405652
CO.[C:3]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O-:21])=[O:20])(=[O:7])[C:4]([CH3:6])=[CH2:5].[Na+:22].[C:23]([NH:27][C:28]([CH3:35])([CH3:34])[CH2:29][S:30]([OH:33])(=[O:32])=[O:31])(=[O:26])[CH:24]=[CH2:25].[OH-].[Na+]>N(C(C)(C)C#N)=NC(C)(C)C#N.CCOCC.O>[C:3]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O-:21])=[O:20])(=[O:7])[C:4]([CH3:6])=[CH2:5].[Na+:22].[C:23]([NH:27][C:28]([CH3:35])([CH3:34])[CH2:29][S:30]([OH:33])(=[O:31])=[O:32])(=[O:26])[CH:24]=[CH2:25]

Komponenten

8

Edukt 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 653602-Acrylamido-2-methyl-1-propanesulfonic acidHCID 87229187Sodium 11-methacrylamidoundecanoate

Produkt 1

HCID 131731611NaMAU AMPSAusbeute 619,5 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6547AzobisisobutyronitrileKatalysatorHCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Into a mixed solvent of 32.4 mL of methanol and 3.6 mL water (methanol/water=9/1) were dissolved 4.9823 g (17.1 mmol) of sodium 11-methacrylamidoundecanoate (NaMAU), 186.5 mg (0.9 mmol) of 2-acrylamido-2-methylpropanesulfonic acid (AMPS), 39.6 mg (0.99 mmol) of sodium hydroxide, and 7.4 mg (0.045 mmol) of azobisisobutyronitrile. The solution was deaerated by bubbling argon for 30 minutes, the container was covered with a septum, and the polymerization was conducted by heating the solution at 60° C. for 12 hours. After the completion of the polymerization reaction, the reaction solution was dropwise added into a large excess of ether, and the resulting precipitate was collected by filtration under suction. This precipitate was dissolved in water, dialyzed against pure water for 1 week, and 2.78 g of random NaMAU/AMPS copolymer (95/5) was obtained by freeze-drying (yield: 53.71%).

Aufarbeitung

  1. customby bubbling argon for 30 minutes
  2. customAfter the completion of the polymerization reaction
  3. filtrationthe resulting precipitate was collected by filtration under suction
  4. dissolutionThis precipitate was dissolved in water
  5. customdialyzed against pure water for 1 week

Quellen und Nachweise

ORD-Eintrag
ord-e74563a5dfd343de944fdb3e46ef7ccc
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08753686B2

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