Ammonium Persulfate → (3,5-Dimethyl-4-nitropyridin-2-yl)methanol

HRID 1067033노트

반응식

HRID 1067033 반응식
[CH3:1][C:2]1[CH:3]=[N+:4]([O-])[CH:5]=[C:6]([CH3:11])[C:7]=1[N+:8]([O-:10])=[O:9].S(OC)([O:16][CH3:17])(=O)=O.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>CO.O>[CH3:1][C:2]1[C:3]([CH2:17][OH:16])=[N:4][CH:5]=[C:6]([CH3:11])[C:7]=1[N+:8]([O-:10])=[O:9]

참가 물질

5

반응물 2

HCID 62648Ammonium PersulfateHCID 867570023,5-Dimethyl-4-nitropyridine-N-Oxide dimethyl Sulphate

생성물 1

HCID 4049415(3,5-Dimethyl-4-nitropyridin-2-yl)methanol

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

3,5-Dimethyl-4-nitropyridine-N-Oxide-dimethyl sulfate adduct (VI) (220 gm, 0.75 mole) was dissolved in methanol (1.0 ltr) and the solution heated to reflux. A solution of ammonium persulfate (140 gm) in water (200 ml) was added dropwise over 4 hours after which reflux was continued for 4 hours. Methanol was distilled off under reduced pressure and the residue was basified to pH 10 by addition of caustic lye (105 ml). The mixture was extracted with dichloromethane (2×400 ml). The dichloromethane layer was dried over sodium sulfate and filtered. The product was used as its solution in dichloromethane for the next reaction.

후처리

  1. temperaturethe solution heated to reflux
  2. temperaturereflux
  3. distillationMethanol was distilled off under reduced pressure
  4. additionthe residue was basified to pH 10 by addition of caustic lye (105 ml)
  5. extractionThe mixture was extracted with dichloromethane (2×400 ml)
  6. dry with materialThe dichloromethane layer was dried over sodium sulfate
  7. filtrationfiltered
  8. customThe product was used as its solution in dichloromethane for the next reaction

출처 및 근거

ORD 기록
ord-5a1b70fe1d1b406bb1d67d267201d232
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06245913B1

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