化工社化工社 化学情報印刷レポート · 研究参考用
5-Nitrofurfuryl alcohol → 2-(2-Chlorophenyl)-3-(5-nitro-2-furyl)acrolein
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Nitrofurfuryl alcohol | HCID 17230 | — |
| 反応物 | 1-Chloro-2-(2-methoxyvinyl)benzene | HCID 54178283 | — |
| 触媒 | Boron trifluoride etherate | HCID 8000 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-(2-Chlorophenyl)-3-(5-nitro-2-furyl)acrolein | HCID 54470629 | — |
反応手順
4.0 g of 1-(2-chlorophenyl)-2-methoxyethylene are added dropwise within 20 minutes to 9.55 g of 5-nitrofurfurol in 12 cc of dry benzene at room temperature after the addition of one drop of diethyl ether/trifluoroborane. The mixture is stirred at 35°-40° for 1 hour and is then successively washed with a 5% aqueous sodium acetate solution and water, the benzene solution is dried over magnesium sulphate and concentrated by evaporation. The residue is taken up in 3 cc of concentrated hydrochloric acid, 17 cc of water and 120 cc of glacial acetic acid, and the mixture is stirred at 80°-85° for 3 hours. The mixture is concentrated in a vacuum, and, after cooling, the title compound is obtained as yellow crystals having a M.P. of 148°-151°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03982007 |
| 出典データセット | uspto-grants-1976_09 |
| ORD ID | ord-58b789c282864d8eb44613f4516d772f |
| 出典メモ | uspto-grants-1976_09 |