Thionyl Chloride → 1-Chloromethyl-3-methyl-4-phenylthiobenzene
反応式
O[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:5]([CH3:16])[CH:4]=1.S(Cl)([Cl:19])=O>C(Cl)Cl>[Cl:19][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:5]([CH3:16])[CH:4]=1参加物
4
実験手順
The 1-hydroxymethyl-3-methyl-4-phenylthiobenzene obtained above is dissolved in methylene chloride (100 ml), and thereto is added with stirring thionyl chloride (23.34 ml) under ice cooling. The mixture is stirred for one hour, and the reaction mixture is washed with ice water (100 ml×3), and thereto is added ethyl acetate (500 ml). The mixture is washed in order with 5% aqueous sodium hydrogen carbonate solution (50 ml×4) and saturated aqueous sodium chloride solution (100 ml×2), dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 1-chloromethyl-3-methyl-4-phenylthiobenzene.
後処理
- washthe reaction mixture is washed with ice water (100 ml×3)
- additionis added ethyl acetate (500 ml)
- washThe mixture is washed in order with 5% aqueous sodium hydrogen carbonate solution (50 ml×4) and saturated aqueous sodium chloride solution (100 ml×2)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-2e1f63cb9aee473eb492836264b4855e
- 出典データセット
- uspto-grants-1989_04
- 特許番号
- US04824834
反応ノート
読み込み中…