反応 #72400

ord-544c610998c946a78a2d3f67339e30a4

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONthe solution above was added dropwise to the system at 80° C. over 6 hours in a nitrogen gas atmosphere
  2. 2
    workup.ADDITIONAfter the completion of dropwise addition
  3. 3
    その他to precipitate a polymer
  4. 4
    ろ過followed by filtration
  5. 5
    ろ過The solid collected by filtration
  6. 6
    洗浄was washed
  7. 7
    その他dried under reduced pressure

実験手順

31.63 Gram (0.195 mol) of 4-acetoxystyrene, 13.65 g (0.096 mol) of tert-butyl methacrylate, 2.14 g (0.009 mol) of (4-phenyl)phenyl methacrylate and 3.45 g (0.015 mol) of polymerization initiator V-601 (produced by Wako Pure Chemical Industries, Ltd.) were dissolved in 151.75 g of cyclohexanone. Subsequently, 37.94 g of cyclohexanone was charged into a reaction vessel, and the solution above was added dropwise to the system at 80° C. over 6 hours in a nitrogen gas atmosphere. After the completion of dropwise addition, the reaction solution was stirred for 2 hours, then allowed to cool to room temperature and added dropwise in 2.5 L of hexane to precipitate a polymer, followed by filtration. The solid collected by filtration was washed by splashing 500 mL of hexane thereon and then dried under reduced pressure to obtain 42.68 g of a 4-acetoxystyrene/tert-butyl methacrylate/(4-phenyl)phenyl methacrylate copolymer.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541161B2uspto-grants-2013_09