反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[C:5]([OH:9])[CH:6]=[CH:7][CH:8]=1.Cl[C:13]1[C:18]([Cl:19])=[CH:17][CH:16]=[CH:15][N:14]=1>CN(C)C=O>[Cl:19][C:18]1[C:13]([O:9][C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:10])([F:11])[F:1])[CH:4]=2)=[N:14][CH:15]=[CH:16][CH:17]=1参加物
反応条件
- 温度
- 120 °C
実験手順
20 7.68 g of sodium hydride dispersion (ca. 50 percent in mineral oil) was washed with pentane under nitrogen and 100 ml of N,N-dimethylformamide was then added. 21.92 g (135 mmol) of 3-(trifluoromethyl)phenol was added dropwise over 30 minutes at room temperature. The resultant phenate solution was added dropwise over 2 hours, under nitrogen, to a solution of 20.1 g (136 mmol) of 2,3-dichloropyridine in 80 ml of N,N-dimethylformamide, heated to 120° C. After a reaction time of 3 hours, the mixture was cooled to room temperature, the precipitate of sodium chloride was filtered off and the filtrate was concentrated. The residue was extracted with toluene and 0.1 N hydrochloric acid, and the organic was washed with saturated sodium chloride solution and concentrated. The oily residue was distilled under vacuum. The yield of the title compound was 24.75 g (67 percent) of a colorless oil, content (GC) 99.7 percent. Other data concerning the title compound was:
後処理
- wash20 7.68 g of sodium hydride dispersion (ca. 50 percent in mineral oil) was washed with pentane under nitrogen
- addition100 ml of N,N-dimethylformamide was then added
- temperatureAfter a reaction time of 3 hours, the mixture was cooled to room temperature
- filtrationthe precipitate of sodium chloride was filtered off
- concentrationthe filtrate was concentrated
- extractionThe residue was extracted with toluene and 0.1 N hydrochloric acid
- washthe organic was washed with saturated sodium chloride solution
- concentrationconcentrated
- distillationThe oily residue was distilled under vacuum
出典と根拠
- ORDレコード
- ord-cc8c6adc270f4ed4979afc1d861110b4
- 出典データセット
- uspto-grants-2003_10
- 特許番号
- US06635766B1
関連ノート
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