化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 1,3-Difluoro-5-(2-nitroethenyl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 1-(3,5-Difluorophenyl)-2-nitroethanol | HCID 68562553 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,3-Difluoro-5-(2-nitroethenyl)benzene | HCID 67348789 | 73.2% |
反応手順
Add acetic anhydride (160 mL) to a solution of 1-(3,5-difluorophenyl)-2-nitroethanol (330 g) and 4-dimethylaminopyridine (18 g) in dichloromethane (1000 mL), at room temperature using a water bath to keep the temperature below 35° C. Add acetic acid over 30 min and stir the reaction mixture overnight. Dilute with dichloromethane (660 mL) and wash with 2% aqueous HCl, saturated aqueous sodium chloride, saturated aqueous sodium bicarbonate, dry (magnesium sulfate) and concentrate. Wash the crude with hexanes to give the title compound (220 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07618978B2 |
| 出典データセット | uspto-grants-2009_11 |
| ORD ID | ord-08eabdce62c345299fcf02685759ec39 |
| 出典メモ | uspto-grants-2009_11 |