Thionyl Chloride → 2-(5-(Chloromethyl)pyridin-2-yl)benzonitrile
反応式
O[CH2:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=2[C:11]#[N:12])=[N:7][CH:8]=1.O=S(Cl)[Cl:19]>O1CCOCC1.CCOCC.[Cl-].[Cl-].[Zn+2]>[Cl:19][CH2:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=2[C:11]#[N:12])=[N:7][CH:8]=1参加物
6
反応条件
- 温度
- 0 °C
実験手順
To a cooled (0° C.), stirred solution of 2-[5-(hydroxymethyl)pyridin-2-yl]benzonitrile (4.3 g, 0.020 mol) and ZnCl2 (0.09 g, 0.61 mmol) in p-dioxane (40 mL) was added SOCl2 (1.50 mL, 0.020 mol) dropwise. The mixture was stirred at room temperature for 18 h, diluted with ether, washed with water and brine, dried (MgSO4), and concentrated to give 4.30 g (92%) of product as a brown solid, mp 97°-98° C.
後処理
- washwashed with water and brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-f5efed1e01364d1b8134c6bd04f3e6bc
- 出典データセット
- uspto-grants-1996_03
- 特許番号
- US05498776
反応ノート
読み込み中…