Chlorosulfonic acid → 4-Fluoro-3-nitrobenzene-1-sulfonyl chloride
反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[Cl:11][S:12](O)(=[O:14])=[O:13]>>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:12]([Cl:11])(=[O:14])=[O:13])=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9]参加物
3
反応条件
- 温度
- 100 °C
実験手順
1-Fluoro-2-nitrobenzene (50.0 g, 0.354 mol) was added to chlorosulfonic acid (91 g, 0.778 mol) at 65° C. The resulting mixture was then heated to 100° C. for 18 h. The mixture was cooled to room temperature, poured over ice and extracted with methylene chloride. The combined organic layers were then washed with NaHCO3, then brine, dried over MgSO4, filtered and concentrated in vacuo to afford 4-fluoro-3-nitrobenzenesulfonyl chloride (55.3 g, 65% yield) as a brown oil.
後処理
- temperatureThe mixture was cooled to room temperature
- additionpoured over ice
- extractionextracted with methylene chloride
- washThe combined organic layers were then washed with NaHCO3
- dry with materialbrine, dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-fce13f43402a4465bb523d41adb2d818
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859571B2
反応ノート
読み込み中…