Phosphate → 2-Methoxy-5-(nitromethyl)pyridine

HRID 923481노트

반응식

HRID 923481 반응식
[OH:1][N:2]=[CH:3][C:4]1[CH:5]=[N:6][C:7]([O:10][CH3:11])=[CH:8][CH:9]=1.C(#N)C.P([O-])([O-])([O-])=[O:16].S([O-])(O[O-])(=O)=O.[K+].[K+]>O.CC(C)=O>[CH3:11][O:10][C:7]1[CH:8]=[CH:9][C:4]([CH2:3][N+:2]([O-:16])=[O:1])=[CH:5][N:6]=1

참가 물질

7

반응물 4

HCID 1061PhosphateHCID 6342AcetonitrileHCID 10313463Potassium peroxymonosulphateHCID 765644496-Methoxy-pyridine-3-carboxaldehyde oxime

생성물 1

HCID 1183086842-Methoxy-5-(nitromethyl)pyridine

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

반응 조건

온도
45 °C

실험 절차

To a mixture of 2 g of N-hydroxy-1-(6-methoxypyridin-3-yl)methanimine, 50 ml of acetonitrile, and 50 ml of an aqueous phosphate buffer solution (pH 6.9) was added a mixed liquid of 20 g of potassium peroxymonosulfate (Oxone: 2KHSO5.KHSO4.K2SO4) in 50 ml water and 50 ml of acetone at room temperature, followed by stirring at 45° C. for 4 hours. The insoluble materials were separated by filtration and washed with diethyl ether. The organic layer was washed with a saturated aqueous sodium sulfite solution and a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate, and the solvent was then evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 251 mg of 2-methoxy-5-(nitromethyl)pyridine.

후처리

  1. customThe insoluble materials were separated by filtration
  2. washwashed with diethyl ether
  3. washThe organic layer was washed with a saturated aqueous sodium sulfite solution
  4. dry with materiala saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
  5. customthe solvent was then evaporated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-e882be149f3e41d09377019c46af79cc
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278968B2

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