Acetic Anhydride → 2-(Acetoxymethyl)-4-methoxy-3,5-dimethylpyridine

HRID 35470노트

반응식

HRID 35470 반응식
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[CH3:8][O:9][C:10]1[C:15](C)=[CH:14][N+:13]([O-])=[C:12](C)[C:11]=1[CH3:19]>C(Cl)(Cl)Cl>[C:5]([O:4][CH2:1][C:2]1[C:15]([CH3:14])=[C:10]([O:9][CH3:8])[C:11]([CH3:19])=[CH:12][N:13]=1)(=[O:7])[CH3:6]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 107022374-Methoxy-2,3,5-trimethylpyridine 1-oxide

생성물 1

HCID 50672892-(Acetoxymethyl)-4-methoxy-3,5-dimethylpyridine

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

215 ml of acetic anhydride are added dropwise at room temperature to a solution of 81.5 g of 4-methoxy-2,3,5-trimethylpyridine 1-oxide in 290 ml of chloroform. After boiling under reflux for 4 hours the solution is evaporated, the residue is dissolved in 200 ml of toluene and again evaporated. The residue is taken up in 500 ml of ethyl acetate and shaken out three times with 250 ml of saturated sodium bicarbonate solution. The organic phase is dried over sodium sulphate and evaporated in vacuo. The crude product remaining behind as the residue is chromatographed on 400 g of silica gel with ether. There is obtained (4-methoxy-3,5-dimethyl-2-pyridyl)methyl acetate in the form of an oil.

후처리

  1. temperatureunder reflux for 4 hours the solution
  2. customis evaporated
  3. dissolutionthe residue is dissolved in 200 ml of toluene
  4. customagain evaporated
  5. dry with materialThe organic phase is dried over sodium sulphate
  6. customevaporated in vacuo
  7. customis chromatographed on 400 g of silica gel with ether

출처 및 근거

ORD 기록
ord-328f8c802b774796950eaea93d3cd8a2
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766133

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