Reaktion #171121

Reaktionsgleichung

water

α-methylene-γ-butyrolactone

acrylic acid

sodium dodecyl sulfate

sodium persulfate

sodium hydroxide

water

sodium dodecyl sulfate

→

α-methylene-γ-butyrolactone acrylic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 250 mL round bottom flask equipped with a magnetic stir bar
2. 2
   workup.ADDITIONwas added dropwise over 110 minutes
3. 3
   workup.ADDITIONAfter 10 minutes of monomer mixture addition
4. 4
   workup.ADDITIONwas also added via syringe pump over 110 minutes
5. 5
   workup.ADDITIONAfter both the monomer and aqueous mixtures had added completely
6. 6
   Temperaturafter which the reaction was cooled to room temperature
7. 7
   Sonstigedried under vacuum at 90° C. overnight
8. 8
   SonstigeSize exclusion chromatography yielded a weight average molecular weight of 507 kDa

Vorschrift

To a 250 mL round bottom flask equipped with a magnetic stir bar was added 44.045 g (2.44 mol) water and 0.512 g (1.78×10−3 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture was heated under flowing nitrogen to 74° C., at which time a monomer mixture consisting of 20.805 g (2.13×10−1 mol) α-methylene-γ-butyrolactone that had been previously filtered over basic alumina and 1.100 g (1.83×10−3 mol) acrylic acid was added dropwise over 110 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 83.37 g (4.63 mol) water, 1.32 g (4.58×10−3 mol) sodium dodecyl sulfate (20% aqueous solution), 0.047 g (1.97×10−4 mol) sodium persulfate, and 0.175 g of a 20% aqueous sodium hydroxide solution was also added via syringe pump over 110 minutes. After both the monomer and aqueous mixtures had 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 at 90° C. overnight. Size exclusion chromatography yielded a weight average molecular weight of 507 kDa and a polydispersity of 1.75, relative to polystyrene standards.

Quelle