반응 #710470

ord-af5cc388665046fb9f199acf3b3699c6

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the resulting mixture was heated
  2. 2
    온도refluxed for 19 hours
  3. 3
    기타was returned to room temperature
  4. 4
    농축concentrated under reduced pressure
  5. 5
    기타purified by silica gel column chromatography (hexane:ethyl acetate=19:1)

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09301525B2uspto-grants-2016_04