反応式
C([Li])CCC.[C:6]1([S:12][CH3:13])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[CH3:14][S:15]SC.Cl>CCCCCC.O1CCCC1>[C:6]1([S:12][CH2:13][S:15][CH3:14])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1参加物
反応条件
- 温度
- -70 °C
実験手順
120 ml. of a 1.3M n-butyllithium solution in n-hexane were added dropwise to a solution of 18.8 ml. of thioanisole in 240 ml. of tetrahydrofuran at -20° C. and the reaction mixture was stirred at that temperature for 2 hours. After cooling to -70° C., 16.4 g. of dimethyldisulphide were added to the reaction mixture, which was then stirred at -70° C. for 15 minutes and at room temperature for 1 hour. The reaction mixture was poured into dilute aqueous hydrochloric acid and extracted with ethyl acetate. The extracts were washed with water and an aqueous solution of sodium chloride and concentrated under reduced pressure. The residue was purified by distillation in vacuo to give 18.0 g. of the title compound having the following physical characteristics:
後処理
- extractionextracted with ethyl acetate
- washThe extracts were washed with water
- concentrationan aqueous solution of sodium chloride and concentrated under reduced pressure
- distillationThe residue was purified by distillation in vacuo
- customto give 18.0 g
出典と根拠
- ORDレコード
- ord-97b77afb4189423cbe59a6a3ae2f079d
- 出典データセット
- uspto-grants-1978_12
- 特許番号
- US04128720
関連ノート
読み込み中…