4-Fluorobenzoic Acid → 3-(Chlorosulfonyl)-4-fluorobenzoic acid
反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1>>[Cl:1][S:2]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][C:7]=1[F:6])[C:11]([OH:13])=[O:12])(=[O:5])=[O:3]参加物
3
反応条件
- 温度
- 150 °C
実験手順
Chlorosulphonic acid (100 ml, 1.5 mol) was gradually added to 4-fluorobenzoic acid (43 g, 0.307 mol) with stirring. The clear dark yellow mixture was heated to 150° C. for 24 hours. The yellow solution was cooled back to room temperature and poured onto ice with vigorous stirring. The white precipitate was filtered and pressed dry. The solid was dried overnight in a desiccator under vacuum and over activated silica (54.65 g, 75%). Mp: 116-117° C.; m/z (LC-MS, ESP), RT=4.03 min, (M−−1)=237-239 (ratio 1:3).
後処理
- temperatureThe yellow solution was cooled back to room temperature
- additionpoured onto ice with vigorous stirring
- filtrationThe white precipitate was filtered
- custompressed dry
- customThe solid was dried overnight in a desiccator under vacuum and over activated silica (54.65 g, 75%)
出典と根拠
- ORDレコード
- ord-b5bb2f4675124571b48d8ac00275062e
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07429660B2
反応ノート
読み込み中…