Ethylene Glycol → 3-(Pyridin-4-yloxy)propan-1-OL
反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.[CH2:8]([OH:11])[CH2:9]O.[OH-:12].[Na+].[CH3:14]S(C)=O>>[OH:12][CH2:14][CH2:9][CH2:8][O:11][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1参加物
5
反応条件
- 温度
- 100 °C
実験手順
A mixture of 4-chloropyridine (7 g, 47 mmol), ethylene glycol (17.9 g, 235 mmol) and sodium hydroxide (4.67 g, 195 mmol) in DMSO (80 ml) was heated at 100° C. for 24 hours. Most of the solvent was removed by evaporation and the residue was diluted with ice water. The aqueous mixture was extracted with ethyl acetate, the extracts combined, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by column chromatography eluting with methylene chloride/methanol mixtures (100/0 increasing to 97/3) to give 4-(3-hydroxypropoxy)pyridine (3.2 g, 45%).
後処理
- customMost of the solvent was removed by evaporation
- additionthe residue was diluted with ice water
- extractionThe aqueous mixture was extracted with ethyl acetate
- dry with materialdried (MgSO4)
- customthe solvent removed by evaporation
- customThe residue was purified by column chromatography
- washeluting with methylene chloride/methanol mixtures (100/0 increasing to 97/3)
出典と根拠
- ORDレコード
- ord-f61e2bab27ce48c1969a1fd50296fb40
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05962458
反応ノート
読み込み中…