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

HRID 35470ノート

反応式

HRID 35470 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](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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-328f8c802b774796950eaea93d3cd8a2
出典データセット
uspto-grants-1988_08
特許番号
US04766133

反応ノート

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