반응 #171138

반응 방정식

4-vinyl benzoic acid

sodium persulfate

water

α-methylene-γ-butyrolactone

water

hydroxyethyl methacrylate

→

α-methylene-γ-butyrolactone hydroxyethyl methacrylate 4-vinyl benzoic acid

반응 조건

후처리

1. 1
   기타To a 250 mL round bottom flask equipped with a magnetic stir bar
2. 2
   workup.ADDITIONis added via syringe pump over 180 minutes
3. 3
   온도at reflux
4. 4
   workup.ADDITIONAfter 10 minutes of monomer mixture addition
5. 5
   workup.ADDITIONis added via syringe pump over 180 minutes
6. 6
   온도at reflux
7. 7
   workup.ADDITIONAfter both the monomer and aqueous mixtures are completely added
8. 8
   온도to cool to room temperature
9. 9
   기타dried under vacuum at elevated temperature for isolation

실험 절차

To a 250 mL round bottom flask equipped with a magnetic stir bar is added 50 g (2.78 mol) water and 1.67 g of the surfactant Abex EP-110 (Rhodia). The mixture is heated under flowing nitrogen to 75° C., at which time a monomer mixture consisting of 14.70 g (1.50×10−1 mol) α-methylene-γ-butyrolactone, 19.55 g (1.50×10−1 mol) hydroxyethyl methacrylate, and 1.71 g (1.16×10−2 mol) 4-vinyl benzoic acid is added via syringe pump over 180 minutes at reflux. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 16.667 g (0.925 mol) water, 0.12 g (5.04×10−4 mol) sodium persulfate, is added via syringe pump over 180 minutes at reflux. After both the monomer and aqueous mixtures are completely added, the emulsion is allowed to stir for an additional 60 minutes, after which the reaction is allowed to cool to room temperature and dried under vacuum at elevated temperature for isolation.

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