反応 #8657

反応方程式

2-Methyladamantanyl methacrylate

methacrylonitrile

alpha-butyrolactone methacrylate

VAZO67

→

2-methyladamantanylmethacrylate methacrylonitrile alpha-butyrolactone Methacrylate

溶媒

—

hexanes

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   その他The resulting colorless solution was deoxygenated
2. 2
   その他by gently bubbling a stream of N2 through the stirring solution for 15 minutes
3. 3
   workup.ADDITIONwas then added to the refluxing mixture over 10 minutes
4. 4
   温度The polymerization was then refluxed
5. 5
   温度cooled to room temperature
6. 6
   ろ過filtered
7. 7
   その他dried
8. 8
   workup.DISSOLUTIONre-dissolved in 70 mL of tetrahydrofuran
9. 9
   その他precipitated into 800 mL of hexanes
10. 10
    ろ過filtered
11. 11
    洗浄washed well with hexanes
12. 12
    その他dried in a vacuum oven at 40° C. for 24 hours

実験手順

2-Methyladamantanyl methacrylate (14.21 g, 0.061 mol), methacrylonitrile (3.05 g, 0.045 mol), and alpha-butyrolactone methacrylate (7.74 g, 0.045 mol) were dissolved in 66 mL of tetrahydrofuran. The resulting colorless solution was deoxygenated by gently bubbling a stream of N2 through the stirring solution for 15 minutes, placed under N2, and heated to 90° C. (oil bath temperature). VAZO67 (0.58 g, 0.0030 mol) dissolved in 7 ml of tetrahydrofuran, was then added to the refluxing mixture over 10 minutes. The polymerization was then refluxed with stirring for 20 hours and cooled to room temperature. The polymer was isolated by precipitation into 800 mL of hexanes, filtered, dried, re-dissolved in 70 mL of tetrahydrofuran, precipitated into 800 mL of hexanes, filtered, washed well with hexanes, and dried in a vacuum oven at 40° C. for 24 hours. Yield 19.8 g (79% of theory). Composition of the title terpolymer was determined by quantitative C-13 NMR and was found to be within experimental error of the monomer feed ratio.

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