反应详情

A dried reaction flask equipped for magnetic stirring was flushed with nitrogen and charged with 2,6,6-trimethyl-5,5-bis(trimethylsilyl)-5,6-disilaheptan-2-ol (53.6 g, 160 mmol, prepared as described in Example 1) and dry tetrahydrofuran (400 mL). Triethylamine (78.1 mL, 56.7 g, 560 mmol) and methacryloyl chloride (54.7 mL, 58.5 g, 560 mmol) were added, and the reaction mixture was stirred at room temperature for 24 hours. Analysis of the reaction mixture by gas chromatography indicated the clean formation of a single product. Pentane (500 mL) was added, precipitated triethylamine hydrochloride was separated by filtration, and the filtrate was concentrated under reduced pressure. The turbid concentrate was dissolved in pentane (500 mL), the resultant solution was filtered and concentrated under reduced pressure, and 2,6-di-tert-butyl-4-methylphenol (0.50 g, 2.3 mmol) was added to the concentrate. The concentrate was distilled under vacuum (bp 120-130° C. at 0.05 mm) to afford the title compound (43.5 g, 67%) as a clear, colorless liquid. The distilled product was characterized by the following NMR data: 1H NMR (CDCl3) δ 0.13 (s, 27 H), 0.70-0.80 (m, 2 H), 1.43 (s, 6 H), 1.75-1.85 (m, 2 H), 1.87 (s, 3 H), 5.43 (m, 1 H), 5.96 (m, 1 H); 13C NMR (CDCl3) δ 0.78 (1 C), 0.99 (9 C), 18.30 (1 C), 25.19 (2 C), 40.25 (1 C), 82.83 (1 C), 123.89 (1 C), 137.85 (1 C), 166.36 (1 C); 29Si NMR (CDCl3) δ −81.26 (1 Si), −12.80 (3 Si).

1. customA dried reaction flask
2. customequipped
3. customwas flushed with nitrogen
4. stirringthe reaction mixture was stirred at room temperature for 24 hours
5. customprecipitated triethylamine hydrochloride
6. customwas separated by filtration
7. concentrationthe filtrate was concentrated under reduced pressure
8. concentrationThe turbid concentrate
9. dissolutionwas dissolved in pentane (500 mL)
10. filtrationthe resultant solution was filtered
11. additionwas added to the concentrate
12. distillationThe concentrate was distilled under vacuum (bp 120-130° C. at 0.05 mm)