反应详情

温度

77 °C

A stirred mixture of trimethylsilylcrotonate (131 g, 0.828 mol), N-bromosuccinimide (206 g, 1.16 mol), benzoyl peroxide (3.41 g, 0.141 mol) and carbon tetrachloride (1 L) is warmed to reflux (77° C.) under visible light for 5 hours. The mixture is cooled to room temperature and the precipitated solid is removed by filtration. The filtrate is concentrated to a residue, which is distilled under reduced pressure. The product fractions are collected at 93–106° C. (9–15 mmHg) to give 127 g of the title compound (65%). GC-MS purity is 83–89%, 1HNMR is consistent with expected structure.

1. temperatureis warmed
2. temperatureThe mixture is cooled to room temperature
3. customthe precipitated solid is removed by filtration
4. concentrationThe filtrate is concentrated to a residue, which
5. distillationis distilled under reduced pressure
6. customThe product fractions are collected at 93–106° C. (9–15 mmHg)