反応式
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11].C(=O)([O-])[O-].[K+].[K+].C1(C)C=CC(S(O[CH:29]2[CH2:33][CH2:32][CH2:31][CH2:30]2)(=O)=O)=CC=1>C(#N)C>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH:29]2[CH2:33][CH2:32][CH2:31][CH2:30]2)=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11]参加物
実験手順
A solution of 2-fluoro-4-chloro-5-hydroxynitrobenzene (7.1 g, 37.1 mmol) and potassium carbonate (5.1 g, 37.1 mmol) in acetonitrile (300 ml) was stirred for 2 hours at a refluxing temperature. Cyclopentyl p-toluenesulfonate (10.3 g, 40.8 mmol) was added thereto, followed by stirring further for 2 hours under refluxing. After completion of the reaction, the solvent was distilled off under reduced pressure from the reaction mixture, in hydrochloric acid (300 ml) was added thereto, and the mixture was extracted with ethyl acetate (100 ml×3 times). The organic layer was washed with an aqueous solution of sodium bicarbonate and water, dried, and the solvent was distilled off under reduced pressure to obtain 2-fluoro-4-chloro-5-cyclopentyloxynitrobenzene as a yellow solid (8.93 g, 34.3 mmol, 92.6% yield).
後処理
- temperatureunder refluxing
- customAfter completion of the reaction
- distillationthe solvent was distilled off under reduced pressure from the reaction mixture, in hydrochloric acid (300 ml)
- additionwas added
- extractionthe mixture was extracted with ethyl acetate (100 ml×3 times)
- washThe organic layer was washed with an aqueous solution of sodium bicarbonate and water
- customdried
- distillationthe solvent was distilled off under reduced pressure
出典と根拠
- ORDレコード
- ord-0b1ea39f652a4ec0b1ad722b5587f73d
- 出典データセット
- uspto-grants-1995_06
- 特許番号
- US05424277
関連ノート
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