Azobisisobutyronitrile → (4-((2,2-Difluoro-3-(methacryloyloxy)propanoyl)oxy)phenyl)diphenylsulfonium perfluorobutanesulfonate

関与物質

反応手順

20.0 mmol of Vazo® 52 low-temperature polymerization initiator (E. I. du Pont de Nemours and Company) is added to a solution of 35.7 g (152.3 mmol) 2-methyl-2-adamantyl methacrylate, 25.9 g (152.3 mmol) 2-methyl-acrylic acid 2-oxo-tetrahydro-furan-3-yl ester, 17.4 g (76.2 mmol) hydroxynaphthylmethyl acrylate and 15.1 g (20.0 mmol) of the 4-((2,2-difluoro-3-(methacryloyloxy)propanoyl)oxy)phenyl)diphenylsulfonium perfluorobutanesulfonate in a 100 g acetonitrile:tetrahydrofuran 2:1 mixture. The monomers and initiator solution are degassed for 10 minutes. Under inert atmosphere, 5 mL of the monomer and initiator solution are introduced into a reactor which is preheated to 80° C. (oil bath). The remainder of the monomer and initiator mixture is fed into the reactor at 80° C. over a two hour period. Upon completion of the addition, the reaction mixture is refluxed for two additional hours. The mixture is next cooled to room temperature and the polymerization solution is precipitated into a large amount of diisopropyl ether, filtered and is then dried under vacuum. The resulting crude polymer is dissolved in 25-30 wt % tetrahydrofuran (THF) and precipitated into diisopropyl ether. The precipitated polymer is isolated by filtration and dried overnight at 40° C. under vacuum. The monomer structures for the polymeric bond PAG are summarized in following table.

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