Azobisisobutyronitrile → 3-Methoxy-2-nitro-6-pyridylmethyl bromide

HRID 622708

반응식

HRID 622708 반응식
N(C(C)(C)C#N)=NC(C)(C)C#N.[CH3:13][O:14][C:15]1[C:16]([N+:22]([O-:24])=[O:23])=[N:17][C:18]([CH3:21])=[CH:19][CH:20]=1.[Br:25]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[CH3:13][O:14][C:15]1[C:16]([N+:22]([O-:24])=[O:23])=[N:17][C:18]([CH2:21][Br:25])=[CH:19][CH:20]=1

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 27279653-Methoxy-6-methyl-2-nitropyridine

생성물 1

HCID 144051243-Methoxy-2-nitro-6-pyridylmethyl bromide수율 21.3%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

A catalytic amount of α,α'-azobis(isobutyronitrile) was added to 3-methoxy-6-methyl-2-nitropyridine (described in Acta Chem. Scand., vol. 23, pages 1791-1796) (7.1 g), N-bromosuccinimide (7.1 g) and carbon tetrachloride (80 ml), and the mixture was refluxed for 16 hours. After the reaction, while the reaction mixture was still hot, it was suction-filtered to separate the insoluble succinimide. The filtrate was cooled to room temperature whereupon the unreacted 3-methoxy-6-methyl-2-nitropyridine precipitated as crystals. The crystals were separated by filtration. The residue was concentrated and then vacuum distilled to give 3-methoxy-2-nitro-6-pyridylmethyl bromide (2.1 g).

후처리

  1. temperaturethe mixture was refluxed for 16 hours
  2. customAfter the reaction
  3. filtrationit was suction-filtered
  4. customto separate the insoluble succinimide
  5. customprecipitated as crystals
  6. customThe crystals were separated by filtration
  7. concentrationThe residue was concentrated
  8. distillationvacuum distilled

출처 및 근거

ORD 기록
ord-f9c7e3be90e044b4ae9244e313e2dd74
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772620

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