反应详情

温度

50 °C

To a suspension of 150 g of methyl p-toluate and 195.5 g of NBS in CCl4 (1.67 L) under N2 at 50° C. was added portion wise over 30 min, solid benzoyl peroxide (5.0 g). There was no exothermic reaction observed. After heating for 2 hours at 50° C., the yellow solution was heated at 65° C. for 6 hrs. There was still some unreacted starting material. The suspension was stirred overnight at 65° C. After cooling to room temperature (r.t), the precipitate formed was filtered off and washed with 150 mL of CCl4 and the filtrate was concentrated to afford a yellow oil that solidified on standing. The title compound, containing a small fraction of starting material was used in the next step without further purification.

1. additionwas added portion wise over 30 min
2. customno exothermic reaction
3. temperaturethe yellow solution was heated at 65° C. for 6 hrs
4. temperatureAfter cooling to room temperature (r.t)
5. customthe precipitate formed
6. filtrationwas filtered off
7. washwashed with 150 mL of CCl4
8. concentrationthe filtrate was concentrated
9. customto afford a yellow oil that solidified