反应 #710470

ord-af5cc388665046fb9f199acf3b3699c6

反应方程式

Cc1ccc(Br)nc1
2-bromo-5-methylpyridine
O=C1CCC(=O)N1Br
N-bromosuccinimide
BrCc1ccc(Br)nc1
2-bromo-5-bromomethylpyridine
收率 20.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the resulting mixture was heated
  2. 2
    温度refluxed for 19 hours
  3. 3
    其他was returned to room temperature
  4. 4
    浓缩concentrated under reduced pressure
  5. 5
    其他purified by silica gel column chromatography (hexane:ethyl acetate=19:1)

实验过程

500 mg (2.92 mmol) of 2-bromo-5-methylpyridine was dissolved in 15 ml of carbon tetrachloride, 623 mg (3.50 mmol) of N-bromosuccinimide and 10 mg of benzoyl peroxide were added thereto, and the resulting mixture was heated and refluxed for 19 hours. After the reaction was completed, the reaction solution was returned to room temperature, concentrated under reduced pressure and purified by silica gel column chromatography (hexane:ethyl acetate=19:1) to obtain 143 mg (yield 20%) of 2-bromo-5-bromomethylpyridine.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09301525B2uspto-grants-2016_04