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2-Amino-5-bromo-3-methylpyridine → HCID 178422464, 화합물

HRID 393776
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HRID 393776 반응식
N[C:2]1[C:7]([CH3:8])=[CH:6][C:5]([Br:9])=[CH:4][N:3]=1.N([O-])=[O:11].[Na+]>OS(O)(=O)=O.O>[Br:9][C:5]1[CH:6]=[C:7]([CH3:8])[C:2]([OH:11])=[N:3][CH:4]=1
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참가 물질

5

반응물 2

HCID 1379342-Amino-5-bromo-3-methylpyridineHCID 23668193Sodium Nitrite

생성물 1

HCID 178422464HCID 178422464, 화합물수율 84%

시약·촉매·용매 2

HCID 962Water용매HCID 1118Sulfuric Acid용매

실험 절차

2-Amino-5-bromo-3-methylpyridine (5.0 g, 26.7 mmol) in 2.6M H2SO4 (70 mL) was treated with sodium nitrite (5.0 g, 72.5 mmol) in water (10 mL) dropwise at 0° C. The mixture was allowed to warm to ambient temperature and stir for 1.5 hours. The mixture was filtered and the filtercake washed with cold water. The filtercake was dissolved in dichloromethane (100 mL), dried (MgSO4), and concentrated to provide the title compound (4.2 g, 84% yield). MS (DCI/NH3) M/z 188/190 (M+H)+.

후처리

  1. filtrationThe mixture was filtered
  2. washthe filtercake washed with cold water
  3. dissolutionThe filtercake was dissolved in dichloromethane (100 mL)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b215675b2fac4e29878af11d8c1f0757
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06809105B2

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