Thionyl Chloride → HCID 58566473、化合物
反応式
S(Cl)([Cl:3])=O.[CH3:5][C:6]1[S:10][C:9]2[C:11]([CH2:15]O)=[CH:12][CH:13]=[CH:14][C:8]=2[CH:7]=1>ClCCl>[Cl:3][CH2:15][C:11]1[C:9]2[S:10][C:6]([CH3:5])=[CH:7][C:8]=2[CH:14]=[CH:13][CH:12]=1参加物
4
実験手順
Thionyl chloride (0.415 mL, 5.69 mmol) was added slowly to an ice cold solution of the alcohol (510) (0.203 g, 1.14 mmol) in dichloromethane (6.0 mL). The reaction mixture was stirred and warmed to room temperature for 1 h. The resulting solution was quenched slowly with saturated sodium bicarbonate (10 mL) and extracted with dichloromethane, the organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo to provide the intermediate 7-(chloromethyl)-2-methylbenzo[b]thiophene (511) (0.150 g, 67.0%) as a yellow oil.
後処理
- customThe resulting solution was quenched slowly with saturated sodium bicarbonate (10 mL)
- extractionextracted with dichloromethane
- dry with materialthe organic layer was dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-14b10aa089344246b9d3ef673c81a1a7
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08309600B2
反応ノート
読み込み中…