Acetic Acid → (4-Methylpyridin-2-yl)methyl acetate

HRID 1091048ノート

反応式

HRID 1091048 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N:3]=1.OO.C(=O)([O-])[O-].[Na+].[Na+].[C:17]([OH:20])(=[O:19])[CH3:18]>>[CH3:8][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([CH2:1][O:20][C:17](=[O:19])[CH3:18])[CH:7]=1

参加物

5

反応物 4

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 79362,4-DimethylpyridineHCID 10340Sodium Carbonate

生成物 1

HCID 19912996(4-Methylpyridin-2-yl)methyl acetate

実験手順

24.3 ml of 2,4-dimethylpyridine were dissolved in 80 ml of glacial acetic acid, the solution was mixed with 30 ml of 30% hydrogen peroxide and refluxed for 25 hours. The solution was then adjusted to approximately pH 8 with saturated sodium carbonate solution, the solution was extracted with dichloromethane and the organic phase rotated in. The residue was mixed with 90 ml of acetic anhydride and refluxed for 1.5 hours. The pH-value of the solution was adjusted to approximately 8 with 40% NaOH and the solution was extracted with trichloromethane. 30 g of crude 4-methyl-2-acetoxymethylpyridine were obtained.

後処理

  1. temperaturerefluxed for 25 hours
  2. extractionthe solution was extracted with dichloromethane
  3. additionThe residue was mixed with 90 ml of acetic anhydride
  4. temperaturerefluxed for 1.5 hours
  5. extractionthe solution was extracted with trichloromethane

出典と根拠

ORDレコード
ord-b2890180fe084e2191616b28c0c3b636
出典データセット
uspto-grants-1992_01
特許番号
US05084458

反応ノート

読み込み中…