Reaction #56350

ord-64a9bf2ab9ad4033bab0329dec4fa910

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.ADDITIONwas charged under nitrogen with 4000 ml
  2. 2
    OtherIt was then sealed
  3. 3
    OtherThe subsequent copolymerization at 25° C.
  4. 4
    Otherabout two hours
  5. 5
    OtherThe reaction was quenched by addition of one liter of diethyl ether
  6. 6
    OtherVolatiles were removed by steam-stripping in a well-ventilated hood
  7. 7
    OtherThe terpolymer thereby obtained
  8. 8
    Otherprecipitated in water in a blender
  9. 9
    Otheroven-dried

Procedure

A 7.57-liter stirred autoclave was charged under nitrogen with 4000 ml. of methylene chloride, 400 grams of ethyl acrylate, 20 grams of maleic anhydride, 1.2 grams of allyl acrylate, and 1.0 gram of azobis(isobutyronitrile). It was then sealed, charged with 300 grams of boron trifluoride, and pressured to 21 kg./sq. cm. with ethylene. The subsequent copolymerization at 25° C. was continued until pressure measurement indicated that ethylene uptake had ceased (about two hours later). The reaction was quenched by addition of one liter of diethyl ether. Volatiles were removed by steam-stripping in a well-ventilated hood. The terpolymer thereby obtained was dissolved in acetone, precipitated in water in a blender, and oven-dried. Yield: 415 grams.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04225476uspto-grants-1980_09