関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Chloro-1-fluoro-4-nitrobenzene | HCID 67688 | — |
| 反応物 | 3-Methoxy-2-pyridone | HCID 88731 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-(2-Chloro-4-nitrophenyl)-3-methoxypyridin-2(1H)-one | HCID 59586748 | — |
反応手順
15 g (120 mmol) of 3-methoxypyridone are dissolved in 120 ml of anhydrous dimethyl sulfoxide and admixed with 16.1 g (144 mmol) of potassium tert-butoxide with stirring. After 30 min, 21.0 g (120 mmol) of 3-chloro-4-fluoronitrobenzene are added and the mixture is heated to 80° C. After 16 h, the mixture is allowed to cool, admixed with 1N hydrochloric acid and extracted repeatedly with dichloromethane. The combined dichloromethane phases are washed with water and saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated to dryness under reduced pressure. The resulting residue is stirred with tert-butyl methyl ether and filtered. The solid is dried under reduced pressure. 22.8 g (60% of theory) of the desired compound are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08198267B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-968b7a033bb046329421c1ce765e1eb2 |
|---|
| 出典メモ | uspto-grants-2012_06 |
|---|