Reaktion #171132

Reaktionsgleichung

water

α-methylene-γ-butyrolactone

N,N-dimethyl acrylamide

sodium dodecyl sulfate

sodium persulfate

sodium hydroxide

water

sodium dodecyl sulfate

→

α-methylene-γ-butyrolactone N,N-dimethyl acrylamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 100 mL round bottom flask equipped with a magnetic stir bar
2. 2
   workup.ADDITIONwas added via syringe pump over 120 minutes
3. 3
   workup.ADDITIONAfter 10 minutes of monomer mixture addition
4. 4
   workup.ADDITIONwas added via syringe pump over 120 minutes
5. 5
   workup.ADDITIONAfter both the monomer and aqueous mixtures were added completely
6. 6
   Temperaturafter which the reaction was cooled to room temperature
7. 7
   Sonstigedried under vacuum under vacuum at 90° C. overnight
8. 8
   SonstigeSize exclusion chromatography yielded a monomodal peak with a weight average molecular weight of 200 kDa
9. 9
   Sonstigeat approximately 162° C.

Vorschrift

To a 100 mL round bottom flask equipped with a magnetic stir bar was added 8.844 g (0.491 mol) water and 0.121 g (4.20×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture was heated under flowing nitrogen to 73° C., at which time a monomer mixture consisting of 2.053 g (2.09×10−2 mol) α-methylene-γ-butyrolactone and 2.113 g (2.13×10−2 mol) N,N-dimethyl acrylamide was added via syringe pump over 120 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 16.658 g (0.925 mol) water, 0.264 g (9.15×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.029 g (1.22×10−4 mol) sodium persulfate, and 0.028 g of a 20% aqueous sodium hydroxide solution was added via syringe pump over 120 minutes. After both the monomer and aqueous mixtures were added completely, the emulsion was allowed to stir for an additional 60 minutes, after which the reaction was cooled to room temperature and dried under vacuum under vacuum at 90° C. overnight. Size exclusion chromatography yielded a monomodal peak with a weight average molecular weight of 200 kDa and a polydispersity of 3.32, relative to polystyrene standards. Differential scanning calorimetry showed a first order transition at approximately 162° C.

Quelle