反应详情

温度

25 °C

Into the 200 ml jacketed reactor described in Example II were added 15.0 grams (0.127 m) alpha-methylstyrene, 15.5 grams (0.1 m) 67.3% t-amyl hydroperoxide and 3.8 grams (0.041 m) phenol. The mixture was stirred to obtain a clear solution and the temperature was adjusted to 20° C. by pumping cool water through the reactor jacket. To this solution was added 1.4 grams (0.009 m) of t-cumyl chloride from the addition funnel over 10 minutes while holding the temperature at 21°-22° C. The reaction was stirred 5 minutes at 22° C., the temperature raised to 25° C. and the reaction stirred 1/2 hour at 30° C., 1/2 hour at 35° C., 11/2 hours at 40° C. and 1/2 hour at 45° C. for a total reaction time of 31/2 hours. At this point essentially all the t-amyl hydroperoxide had been consumed. The reaction was terminated by adding 25 mls of water, stirring 5 minutes, adding 5 mls of 50% NaOH, stirring another 5 minutes and then separating the aqueous caustic layer. The organic layer was washed with saturated NaHCO3 solution, water, 15% NaHSO3, saturated NaHCO3 again and water. The dried material weighed 24.6 grams and contained 54.6% cumyl t-amyl peroxide for a corrected yield of 13.4 grams and a 60.5% yield. The pure cumyl t-amyl peroxide was isolated by fractional distillation under vacuum.

1. customto obtain a clear solution
2. customwas adjusted to 20° C.
3. customat 21°-22° C
4. stirringThe reaction was stirred 5 minutes at 22° C.
5. stirringthe reaction stirred 1/2 hour at 30° C., 1/2 hour at 35° C.
6. custom2 hours
7. customat 40° C.
8. custom1/2 hour
9. customat 45° C.
10. customAt this point essentially all the t-amyl hydroperoxide had been consumed
11. customThe reaction was terminated
12. additionby adding 25 mls of water
13. stirringstirring 5 minutes
14. additionadding 5 mls of 50% NaOH
15. stirringstirring another 5 minutes
16. customseparating the aqueous caustic layer
17. washThe organic layer was washed with saturated NaHCO3 solution, water, 15% NaHSO3, saturated NaHCO3 again