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Methanol → 2,6-Dibromo-4-methoxypyridine

HRID 1908821
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HRID 1908821 반응식
[CH3:1][OH:2].[H-].[Na+].[Br:5][C:6]1[CH:11]=[C:10]([N+]([O-])=O)[CH:9]=[C:8]([Br:15])[N:7]=1>>[Br:5][C:6]1[CH:11]=[C:10]([O:2][CH3:1])[CH:9]=[C:8]([Br:15])[N:7]=1
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참가 물질

4

반응물 3

HCID 887MethanolHCID 24758Sodium hydrideHCID 160387482,6-Dibromo-4-nitropyridine

생성물 1

HCID 109015692,6-Dibromo-4-methoxypyridine수율 68.1%

실험 절차

Methanol (1.48 g, 46.1 mmol) is slowly added to a cooled suspension (0° C.) of NaH (2.12 g, 53.2 mmol, 60% dispersion in mineral oil, washed with hexane prior to use) in THF (20 mL). Upon completion of the addition the mixture is stirred at 0° C. for 150 min before 2,6-dibromo-4-nitropyridine (10.0 g, 35.4 mmol) is added. The temperature rises to 14° C. The mixture is stirred at rt for 3 h before the reaction is quenched with sat. aq. NH4Cl solution. The mixture is diluted with water and extracted twice with EA (250 mL). The combined org. extracts are dried over MgSO4, filtered and concentrated. The crude product is purified by CC on silica gel eluting with DCM to give 2,6-dibromo-4-methoxy-pyridine (6.43 g) as an off-white solid; LC-MS: tR=0.90 min, [M+1]+=267.75.

후처리

  1. washwashed with hexane
  2. additionUpon completion of the addition the mixture
  3. additionis added
  4. customrises to 14° C
  5. customis quenched with sat. aq. NH4Cl solution
  6. additionThe mixture is diluted with water
  7. extractionextracted twice with EA (250 mL)
  8. dry with materialextracts are dried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe crude product is purified by CC on silica gel eluting with DCM

출처 및 근거

ORD 기록
ord-d7da940b1fc84bff8d4cd5288482af3c
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598208B2

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