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

HRID 979872ノート

反応式

HRID 979872 の反応式
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[CH2:8]([O:10][C:11]1[C:16]([CH3:17])=[CH:15][N+:14]([O-])=C(C)[CH:12]=1)[CH3:9]>C(Cl)(Cl)Cl>[C:5]([O:4][CH2:1][C:2]1[CH:12]=[C:11]([O:10][CH2:8][CH3:9])[C:16]([CH3:17])=[CH:15][N:14]=1)(=[O:7])[CH3:6]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 221514414-Ethoxy-2,5-dimethylpyridine 1-oxide

生成物 1

HCID 22151443(4-Ethoxy-5-methyl-2-pyridyl)methyl acetate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

20 ml of acetic anhydride were added dropwise at room temperature to a solution of 7.8 g of 4-ethoxy-2,5-dimethylpyridine 1-oxide in 30 ml of chloroform. After boiling under reflux for 3 hours the solution was evaporated, the residue was dissolved in 50 ml of toluene and again evaporated. The residue was taken up in 50 ml of ethyl acetate, whereupon the solution was extracted three times with 20 ml of saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and evaporated in vacuo. The product was chromatographed on 50 g of silica gel with ether and there was obtained (4-ethoxy-5-methyl-2-pyridyl)methyl acetate in the form of an oil.

後処理

  1. temperatureunder reflux for 3 hours the solution
  2. customwas evaporated
  3. dissolutionthe residue was dissolved in 50 ml of toluene
  4. customagain evaporated
  5. extractionwas extracted three times with 20 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 50 g of silica gel with ether

出典と根拠

ORDレコード
ord-55fdad801e6d4691bc66ee348fa65cdf
出典データセット
uspto-grants-1987_01
特許番号
US04634710

反応ノート

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