反応式
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[F:10][C:11]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[C:12]=1[C:13]([OH:15])=[O:14].O>ClCCl>[F:10][C:11]1[C:12]([C:13]([OH:15])=[O:14])=[C:16]([C:20]([F:21])([F:22])[F:23])[C:17]([N+:1]([O-:4])=[O:2])=[CH:18][CH:19]=1参加物
6
反応条件
- 温度
- 0 °C
実験手順
1.05 ml (23.3 mmol) of concentrated nitric acid (65%), which also was precooled to 0° C., is instilled in a solution of 17.5 ml of concentrated sulfuric acid and 2.5 g (12.0 mmol) of 2-fluoro-6-trifluoromethyl-benzoic acid, cooled to 0° C. It is allowed to stir for one more hour at 0° C. and then overnight at room temperature. It is then poured in a mixture of ice, water and dichloromethane, the organic phase is separated and the aqueous phase is extracted with dichloromethane. The organic solutions are combined, washed with saturated sodium chloride solution, dried on sodium sulfate and evaporated to dryness in a vacuum. The title compound is obtained in crystalline form.
後処理
- customalso was precooled to 0° C.
- customovernight
- customat room temperature
- customthe organic phase is separated
- extractionthe aqueous phase is extracted with dichloromethane
- washwashed with saturated sodium chloride solution
- customdried on sodium sulfate
- customevaporated to dryness in a vacuum
出典と根拠
- ORDレコード
- ord-62788c37a7ea49d1ad1694bc8f5df3e4
- 出典データセット
- uspto-grants-1997_11
- 特許番号
- US05686492
関連ノート
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