反应 #1517

ord-cac03ebf9c0047c583eb8f2217093891

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他a reaction
  2. 2
    温度under reflux for 2 hours
  3. 3
    其他After completion of the reaction
  4. 4
    温度the reaction mixture was cooled in ice bath
  5. 5
    过滤The deposited crystalline product was collected by filtration, which
  6. 6
    洗涤was then washed with hexane and water
  7. 7
    其他by drying
  8. 8
    其他The resultant crystalline product was recrystallized from ethanol
  9. 9
    其他to obtain

实验过程

39.7 g (287 mmol) of p-toluylic acid, 51.2 g (287 mmol) of N-bromosuccinimide and 2.8 g (11.5 mmol) of dibenzoyl peroxide were suspended in 350 ml of carbon tetrachloride. Then, the resultant mixture was heated with vigorously stirring to perform a reaction under reflux for 2 hours. After completion of the reaction, the reaction mixture was cooled in ice bath. The deposited crystalline product was collected by filtration, which was then washed with hexane and water, followed by drying. The resultant crystalline product was recrystallized from ethanol to obtain 40.3 g of 4-bromomethylbenzoic acid as a white needle crystal (isolated yield: 65%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05725798uspto-grants-1998_03