반응 #171127

ord-277d38abaa574fc19bb845ebc2632ccd

반응 조건

온도
75°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타To a 150 mL round bottom flask equipped with a magnetic stir bar
  2. 2
    workup.ADDITIONis added dropwise over 120 minutes
  3. 3
    workup.ADDITIONAfter 5 minutes of monomer mixture addition
  4. 4
    workup.ADDITIONis also added dropwise over 120 minutes
  5. 5
    workup.ADDITIONAfter addition of both the monomer and aqueous mixtures
  6. 6
    온도after which the reaction is cooled to room temperature
  7. 7
    기타the polymer can be dried under vacuum for isolation

실험 절차

To a 150 mL round bottom flask equipped with a magnetic stir bar is added 10.00 g (0.555 mol) water and 0.115 g (3.99×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture is pre-heated under flowing nitrogen to 75° C., at which time a monomer mixture consisting of 4.725 g (4.18×10−2 mol) α-methylene-γ-valerolactone, 0.250 g (4.16×10−3 mol) acrylic acid, and 0.036 g (2.62×10−4 mol) triallyl amine is added dropwise over 120 minutes. After 5 minutes of monomer mixture addition, an aqueous mixture consisting of 18.937 g (1.05 mol) water, 0.300 g (1.04×10−3 mol) sodium dodecyl sulfate (20% aqueous solution), 0.033 g (1.39×10−4 mol) sodium persulfate, and 0.037 g of a 20% aqueous sodium hydroxide solution is also added dropwise over 120 minutes. After addition of both the monomer and aqueous mixtures are complete, the emulsion stirs for an additional 60 minutes, after which the reaction is cooled to room temperature and the polymer can be dried under vacuum for isolation.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846817B2uspto-grants-2014_09