2-Bromoanisole → 3-bromo-4-methoxybenzenesulfonyl chloride
反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][CH3:9].[Cl:10][S:11](O)(=[O:13])=[O:12]>C(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[C:6]([S:11]([Cl:10])(=[O:13])=[O:12])[CH:5]=[CH:4][C:3]=1[O:8][CH3:9]参加物
4
実験手順
1-Bromo-2-methoxy-benzene (1.87 g, 10.0 mmol) was dissolved in chloroform (5 mL) and the solution was cooled in an ice-salt bath to −5° C. to 0° C. The cooled solution was carefully charged with chlorosulfonic acid (2.0 mL, 30.0 mmol) over 30 minutes and the mixture was allowed to warm to room temperature over 1 hour. The mixture then was poured onto chopped ice and transferred to a separatory funnel. The aqueous layer was separated and extracted (×2). The combined organic layers were dried and concentrated to give 3-bromo-4-methoxyphenylsulfonyl chloride (2.80 g, 98%).
後処理
- temperaturethe solution was cooled in an ice-salt bath to −5° C. to 0° C
- additionThe mixture then was poured
- customtransferred to a separatory funnel
- customThe aqueous layer was separated
- extractionextracted (×2)
- customThe combined organic layers were dried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-25becbe87eab498e944dbe1fe6dc2382
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08778625B2
反応ノート
読み込み中…