Reaktion #171131

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 100 mL round bottom flask equipped with a magnetic stir bar
2. 2
   workup.ADDITIONwas added via syringe pump over 135 minutes
3. 3
   workup.ADDITIONAfter 15 minutes of monomer mixture addition
4. 4
   workup.ADDITIONwas added via syringe pump over 135 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 126 kDa
9. 9
   Sonstigeat approximately 174° C.

Vorschrift

To a 100 mL round bottom flask equipped with a magnetic stir bar was added 8.800 g (0.489 mol) water and 0.108 g (3.75×10−4 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 4.103 g (4.18×10−2 mol) α-methylene-γ-butyrolactone and 0.278 g (4.63×10−3 mol) acrylic acid was added via syringe pump over 135 minutes. After 15 minutes of monomer mixture addition, an aqueous mixture consisting of 16.661 g (0.926 mol) water, 0.282 g (9.78×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.034 g (1.43×10−4 mol) sodium persulfate, and 0.032 g of a 20% aqueous sodium hydroxide solution was added via syringe pump over 135 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 126 kDa and a polydispersity of 2.12, relative to polystyrene standards. Differential scanning calorimetry showed a single first order transition at approximately 174° C.

Quelle