Azobisisobutyronitrile → 3,5-Dibromo-2-(bromomethyl)pyridine

HRID 2224349

반응식

HRID 2224349 반응식
[Br:1][C:2]1[C:3]([CH3:9])=[N:4][CH:5]=[C:6]([Br:8])[CH:7]=1.C1C(=O)N([Br:17])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[C:3]([CH2:9][Br:17])=[N:4][CH:5]=[C:6]([Br:8])[CH:7]=1

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 6197053,5-Dibromo-2-methylpyridine

생성물 1

HCID 534171773,5-Dibromo-2-(bromomethyl)pyridine수율 55%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

To a solution of 52A (1.25 g, 4.98 mmol) in CCl4 (7 ML) was added NBS (0.89 g, 4.98 mmol) followed by catalytic AIBN and the mixture was heated to reflux for 4 hours. The reaction was cooled to room temperature, filtered and concentrated in vacuo. The residue was purified by flash chromatography (SiO2, 10% CH2Cl2/Hexane then 50% CH2Cl2/Hexane) to give 52B (0.90 g, 55%). HPLC Rt=2.85 min.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 4 hours
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography (SiO2, 10% CH2Cl2/Hexane

출처 및 근거

ORD 기록
ord-989c30392564450eb7b6d497f16e4150
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07378426B2

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