2-Chlorofuro[3,2-b]pyridine → Furo(3,2-b)pyridine
反応式
Cl[C:2]1[O:10][C:5]2[CH:6]=[CH:7][CH:8]=[N:9][C:4]=2[CH:3]=1>C(O)(=O)C.[Zn]>[O:10]1[C:5]2[CH:6]=[CH:7][CH:8]=[N:9][C:4]=2[CH:3]=[CH:2]1参加物
4
実験手順
Chlorofuropyridine (7, 1.27 g, 8.27 mmol) is treated with zinc (3.23 g, 49.6 mmol) in acetic acid (20 ml) at refluxing temperature until the starting material disappears (˜4 hours). The reaction is filtered to remove solid. The filtrate is concentrated and the residue is dissolved in water. After basification with 1N sodium hydroxide, the mixture is extracted with methylene chloride. Evaporation leaves a yellow oil, which is purified with flash column chromatography on silica gel to give furopyridine as a yellow oil (8).
後処理
- temperatureat refluxing temperature until the starting material
- custom(˜4 hours)
- filtrationThe reaction is filtered
- customto remove solid
- concentrationThe filtrate is concentrated
- dissolutionthe residue is dissolved in water
- extractionAfter basification with 1N sodium hydroxide, the mixture is extracted with methylene chloride
- customEvaporation
- customleaves a yellow oil, which
- customis purified with flash column chromatography on silica gel
出典と根拠
- ORDレコード
- ord-3de1c72e4e3e429ea0e5e5f6958e7d84
- 出典データセット
- uspto-grants-2008_10
- 特許番号
- US07439374B2
反応ノート
読み込み中…