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

HRID 703177
ノート
印刷プレビュー

反応式

HRID 703177 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-435ca48d83024072a1f83af87e05e81a
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04981861

反応ノート

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