Methyl iodide → 3-Methoxy-6-methyl-2-nitropyridine

HRID 529169

반응식

HRID 529169 반응식
[C:1](=O)([O-])[O-].[K+].[K+].CI.[CH3:9][C:10]1[N:15]=[C:14]([N+:16]([O-:18])=[O:17])[C:13]([OH:19])=[CH:12][CH:11]=1.C(OC(=O)C)C>CN(C=O)C.O>[CH3:1][O:19][C:13]1[C:14]([N+:16]([O-:18])=[O:17])=[N:15][C:10]([CH3:9])=[CH:11][CH:12]=1

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 848016-Methyl-2-nitropyridin-3-ol

생성물 1

HCID 27279653-Methoxy-6-methyl-2-nitropyridine수율 78%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

Potassium carbonate (4.15 g) and methyl iodide (2.80 ml) were added to a solution of 6-methyl-2-nitro-3-hydroxypyridine (4.63 g) in DMF (120 ml), and the mixture was stirred at room temperature for 14 hours. The reaction mixture was distributed between ethylacetate and water. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was recrystallized from ethyl acetate/hexane to give the title compound (3.94 g) as needle crystals.

후처리

  1. washThe organic layer was washed with saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe residue was recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-4b37170d3d8f489bb9b6b4722151a99b
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346822B2

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