Thionyl Chloride → 2-(Chloromethyl)-6-methylpyridine
反応式
[CH3:1][C:2]1[N:7]=[C:6]([CH2:8]O)[CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:12])=O>C(Cl)Cl>[Cl:12][CH2:8][C:6]1[CH:5]=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=1参加物
4
実験手順
A solution of (6-methyl-pyridin-2-yl)-methanol (1.44 g, 11.7 mmol), thionyl chloride (1.45 mL, 19.9 mmol) and methylene chloride (20 mL) was stirred under reflux for 40 minutes. The reaction solution was cooled to room temperature and then concentrated under a reduced pressure. The residue was partitioned into sodium bicarbonate solution and diethyl ether. The organic layer was concentrated under a reduced pressure, and the residue was purified by silica gel chromatography (ethyl acetate) to obtain the title compound (1.42 g, 85.8%).
後処理
- temperatureunder reflux for 40 minutes
- concentrationconcentrated under a reduced pressure
- customThe residue was partitioned into sodium bicarbonate solution and diethyl ether
- concentrationThe organic layer was concentrated under a reduced pressure
- customthe residue was purified by silica gel chromatography (ethyl acetate)
出典と根拠
- ORDレコード
- ord-78e6bd01107849bd8231580d44d84968
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841327B2
反応ノート
読み込み中…