反応式
Cl[C:2]1C(Cl)=CC(C(Cl)(Cl)Cl)=C[N:3]=1.Cl[C:14]1[C:19]([Cl:20])=[CH:18][C:17]([C:21]([F:24])([F:23])[F:22])=[CH:16][N:15]=1.[C-]#N.[K+]>CS(C)=O>[Cl:20][C:19]1[C:14]([C:2]#[N:3])=[N:15][CH:16]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:18]=1参加物
実験手順
3-Chloro-2-fluoro-5-(trifluoromethyl)pyridine (obtained as a by-product from the fluorine exchange reaction when converting 2,3-dichloro-5-trichloromethyl pyridine to 2,3-dichloro-5-(trifluoromethyl)pyridine) (40.0 g, 0.2 mole) was put into 270 ml of dimethyl sulfoxide and stirred while potassium cyanide (14.4 g, 0.221 mole) was spooned in over a 20-minute period. The mixture was then stirred for another 20 minutes. The temperature was held between 23° and 28° C. throughout the reaction. The mixture was poured into 600 ml of ice water and the product was extracted into hexane. The hexane was removed on a rotary evaporator. The product was treated with activated charcoal and distilled on a Vigreaux-Claisen still at 108°-110° C. at 30 mm Hg to yield 31.45 g of colorless oil with an analysis of, in percent by weight:
後処理
- customwas spooned in over a 20-minute period
- customThe temperature was held between 23° and 28° C. throughout the reaction
- extractionthe product was extracted into hexane
- customThe hexane was removed on a rotary evaporator
- additionThe product was treated with activated charcoal
- distillationdistilled on a Vigreaux-Claisen still at 108°-110° C. at 30 mm Hg
出典と根拠
- ORDレコード
- ord-83a99c70e02d43f59a316cbf6e75755e
- 出典データセット
- uspto-grants-1990_12
- 特許番号
- USRE033478
関連ノート
読み込み中…