Reaktion #171133

Reaktionsgleichung

acrylic acid

sodium persulfate

water

sodium hydroxide

water

itaconic acid

α-methylene-γ-butyrolactone

→

α-methylene-γ-butyrolactone itaconic acid acrylic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturTo a 100 mL round bottom flask with a magnetic stir bar and reflux condenser
2. 2
   workup.ADDITIONis added via syringe pump over 300 minutes
3. 3
   Temperaturat reflux
4. 4
   workup.ADDITIONAfter 10 minutes of monomer mixture addition
5. 5
   workup.ADDITIONis added via syringe pump over 300 minutes
6. 6
   Temperaturat reflux
7. 7
   workup.ADDITIONAfter both the monomer and aqueous mixtures are added completely
8. 8
   Temperaturbefore cooling to room temperature
9. 9
   Sonstigedrying under vacuum at elevated temperature for isolation

Vorschrift

To a 100 mL round bottom flask with a magnetic stir bar and reflux condenser is added 25 g (1.389 mol) water and 22.75 g (1.75×10−1 mol) itaconic acid. The mixture is heated under flowing nitrogen to 75° C., at which time a monomer mixture consisting of 17.20 g (1.75×10−1 mol) α-methylene-γ-butyrolactone and 2.00 g (3.33×10−2 mol) acrylic acid is added via syringe pump over 300 minutes at reflux. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 18.015 g (1.00 mol) water, 1.42 g (5.97×10−3 mol) sodium persulfate, and 1.32 g (3.33×10−2 mol) sodium hydroxide is added via syringe pump over 300 minutes at reflux. After both the monomer and aqueous mixtures are added completely, the emulsion is allowed to stir for an additional 60 minutes before cooling to room temperature and drying under vacuum at elevated temperature for isolation.

Quelle