Reaktion #721223

ord-6eca4ba767b7418d98bbd75b97c8300b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeafter repeating purging with nitrogen and release of the pressure
  2. 2
    Sonstigesealed in the pressure-reduced state
  3. 3
    SonstigeThis ampule was placed in a constant temperature bath at 50° C.
  4. 4
    Sonstigepolymerization
  5. 5
    SonstigeAfter the completion of polymerization reaction
  6. 6
    Sonstigethe precipitate was vacuum-dried at 80° C. for 10 hours

Vorschrift

A glass ampule having a volume of 75 mL was charged with 50 g (0.25 mol) of diisopropyl fumarate, 15.9 g (0.107 mol) of cinnamic acid and 0.21 g (0.0012 mol) of tert-butyl peroxypivalate as a polymerization initiator and after repeating purging with nitrogen and release of the pressure, sealed in the pressure-reduced state. This ampule was placed in a constant temperature bath at 50° C. and held for 48 hours, thereby performing radical polymerization. After the completion of polymerization reaction, the polymerization product was taken out of the ampule and dissolved in 400 g of tetrahydrofuran. The resulting polymer solution was added dropwise, for precipitation, to 3 L of methanol, and the precipitate was vacuum-dried at 80° C. for 10 hours to obtain 10 g of a diisopropyl fumarate/cinnamic acid copolymer (yield: 15%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09321870B2uspto-grants-2016_04