Acetic Anhydride → 3-octyl-6-(4-octyloxyphenyl)-1H-2-pyridone

HRID 1780543ノート

反応式

HRID 1780543 の反応式
[CH2:1]([C:9]1[CH:10]=[CH:11][C:12]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:18][CH:17]=2)=[N+:13]([O-])[CH:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].C(OC(=O)C)(=[O:33])C>>[CH2:1]([C:9]1[C:14](=[O:33])[NH:13][C:12]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:18][CH:17]=2)=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 543682835-octyl-2-(4-octyloxyphenyl)pyridine N-oxide

生成物 1

HCID 190469563-octyl-6-(4-octyloxyphenyl)-1H-2-pyridone

実験手順

2.20 g (5.4 mmol) of 5-octyl-2-(4-octyloxyphenyl)pyridine N-oxide are refluxed in 30 ml of acetic anhydride for 4 hours. The acetic anhydride is then distilled off, and the residue is taken up in 10 ml of 1:1 methylene chloride/methanol, and the mixture is stirred with methanolic potassium hydroxide solution for 1 hour. Washing with water and concentrated ammonium chloride solution, drying over sodium sulfate, filtration, removal of the solvent by distillation and recrystallization from 8:2 n-hexane/ethyl acetate give 1.79 g of 3-octyl-6-(4-octyloxyphenyl)-1H-2-pyridone. ##STR14##

後処理

  1. distillationThe acetic anhydride is then distilled off
  2. washWashing with water and concentrated ammonium chloride solution
  3. dry with materialdrying over sodium sulfate, filtration, removal of the solvent by distillation and recrystallization from 8:2 n-hexane/ethyl acetate

出典と根拠

ORDレコード
ord-9356afaf2f2f43f28739f6c2a4db3e1d
出典データセット
uspto-grants-1997_05
特許番号
US05630962

反応ノート

読み込み中…