2,3-Dichloropropene → (4-Bromophenyl)(2-chloroallyl)sulfane
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].[Cl:15][C:16]([CH2:18]Cl)=[CH2:17]>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:18][C:16]([Cl:15])=[CH2:17])=[CH:4][CH:3]=1参加物
4
実験手順
According to the procedure of W. K. Anderson et al., J. Chem. Soc., Perkin 1, 1 (1976) a mixture of 4-bromothiophenol (40.0 g, 0.211 mol) and K2CO3 (35.3 g, 0.254 mol) was heated at reflux for 1 hour. 2,3-Dichloro-1-propene (23.5 g, 0.211 mol) was added. The resulting mixture was heated at reflux for 2 hours, cooled and concentrated. The mixture was diluted with H2O and extracted with ether (3×150 mL). The combined extracts were dried (MgSO4), and concentrated to give an oil. Distillation under high vacuum gave 37.2 g (67%) of product as a colorless liquid.
後処理
- temperaturewas heated
- temperatureat reflux for 1 hour
- temperatureThe resulting mixture was heated
- temperatureat reflux for 2 hours
- temperaturecooled
- concentrationconcentrated
- additionThe mixture was diluted with H2O
- extractionextracted with ether (3×150 mL)
- dry with materialThe combined extracts were dried (MgSO4)
- concentrationconcentrated
- customto give an oil
- distillationDistillation under high vacuum
出典と根拠
- ORDレコード
- ord-aabe4721e9b941f08963a1cf7f68b8b1
- 出典データセット
- uspto-grants-1990_01
- 特許番号
- US04895860
反応ノート
読み込み中…