反应详情

To a solution of 2.53 g (2.93 mL, 14.5 mmol) of 1-methoxy-1-trimethylsiloxy-2-methyl-1-propene and 0.5 mL of tetrabutylammonium biacetate (0.1 M in propylene carbonate) in 40 mL of THF was added dropwise a mixture of 29.8 g (33.7 mL, 0.189 mole) of trimethylsilyl methacrylate and 14.5 g (14.5 mL, 0.0582 mole) of ethoxytriethylene glycol methacrylate. The temperature of the reaction mixture rose from 26° C. to 40° C. After addition of an additional 0.5 mL of tetrabutylammonium biacetate (0.1 M in propylene carbonate), the temperature rose to 57° C. When the temperature had fallen to 29° C., 0.3 mL of tetrabutylammonium biacetate (0.1 M in propylene carbonate) was added, followed by 29.9 g (29.6 mL, 0. 157 mole) of 2-phenylethyl methacrylate. The temperature rose to 48° C., and the mixture was stirred overnight. NMR analysis of an aliquot of the reaction mixture showed that there was no residual monomer in the solution of poly(trimethylsilyl methacrylate [46.8 mol %]-co-ethoxytriethylene glycol methacrylate [14.4 mol %]-b-2-phenylethyl methacrylate [38.8 mol %]). The solution was treated with 45 mL of tetrabutylammonium fluoride (0.03 M in methanol) and stirred at reflux for 8 hr. Evaporation under reduced pressure followed by drying in a vacuum oven gave 66.5 g of poly(methacrylic acid [46.8 mol %]-co-ethoxytriethylene glycol methacrylate [14.4 mol %]-b-2-phenylethyl methacrylate [38.8 mol %]).

1. customrose from 26° C. to 40° C
2. customrose to 57° C
3. customhad fallen to 29° C.
4. customrose to 48° C.
5. stirringstirred
6. temperatureat reflux for 8 hr
7. customEvaporation under reduced pressure
8. customby drying in a vacuum oven