Reaktion #492840

Reaktionsgleichung

11-methacrylamidoundecanoic acid

2-dimethylaminoethyl methacrylate

azobisisobutyronitrile

→

MAU 2-dimethylaminoethyl methacrylate

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeby bubbling nitrogen for 60 minutes
2. 2
   SonstigeAfter the completion of the polymerization reaction
3. 3
   Einengenthe solution was concentrated to dryness under reduced pressure
4. 4
   workup.DISSOLUTIONthe solid was dissolved in 60 g of dimethylformamide
5. 5
   workup.ADDITIONThe obtained solution was dropwise added into a large excess of diethyl ether
6. 6
   Filtrationthe resulting precipitate was collected by filtration under suction
7. 7
   SonstigeAfter drying under reduced pressure

Vorschrift

In 59.68 g of methanol were dissolved 18.78 g (69.74 mmol) of 11-methacrylamidoundecanoic acid (MAU), 1.22 g (7.75 mmol) of 2-dimethylaminoethyl methacrylate (Tokyo Chemical industry Co.), and 0.32 g (1.95 mmol) of azobisisobutyronitrile (Nacalai Tesque, Inc.). The solution was deaerated by bubbling nitrogen for 60 minutes. The container was covered with a septum, and the polymerization was conducted by heating at 60° C. for 20 hours. After the completion of the polymerization reaction, the solution was concentrated to dryness under reduced pressure, and the solid was dissolved in 60 g of dimethylformamide. The obtained solution was dropwise added into a large excess of diethyl ether, and the resulting precipitate was collected by filtration under suction. After drying under reduced pressure, 7.78 g of random MAU/2-dimethylaminoethyl methacrylate copolymer (90/10) was obtained (yield: 38.9%). The weight average molecular weight was 250000.

Quelle