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Acetic Anhydride → (4-Methoxy-5-methyl-2-pyridyl)methyl acetate

HRID 979867
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HRID 979867 반응식
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[CH3:8][O:9][C:10]1[C:15]([CH3:16])=[CH:14][N+:13]([O-])=C(C)[CH:11]=1>C(Cl)(Cl)Cl>[C:5]([O:4][CH2:1][C:2]1[CH:11]=[C:10]([O:9][CH3:8])[C:15]([CH3:16])=[CH:14][N:13]=1)(=[O:7])[CH3:6]
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참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 151634614-Methoxy-2,5-dimethylpyridine 1-oxide

생성물 1

HCID 22151432(4-Methoxy-5-methyl-2-pyridyl)methyl acetate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

55 ml of acetic anhydride were added dropwise at room temperature to a solution of 19.9 g of 4-methoxy-2,5-dimethylpyridine 1-oxide in 75 ml of chloroform. After boiling under reflux for 2 hours the solution was evaporated, the residue was dissolved in 100 ml of toluene and again evaporated. The residue was taken up in 100 ml of ethyl acetate and the solution was extracted three times with 50 ml of saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and evaporated in vacuo. The product was chromatographed on 100 g of silica gel with ether and there was obtained (4-methoxy-5-methyl-2-pyridyl)methyl acetate in the form of an oil.

후처리

  1. temperatureunder reflux for 2 hours the solution
  2. customwas evaporated
  3. dissolutionthe residue was dissolved in 100 ml of toluene
  4. customagain evaporated
  5. extractionthe solution was extracted three times with 50 ml of saturated sodium bicarbonate solution
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. customevaporated in vacuo
  8. customThe product was chromatographed on 100 g of silica gel with ether

출처 및 근거

ORD 기록
ord-bbf6d19dcb124e3db962753dfc30d67a
출처 데이터셋
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04634710

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