関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4-Fluoro-2-methoxybenzoic acid | HCID 2774545 | — |
| 生成物 | 4-Fluoro-3-nitro-2-methoxybenzoic acid | HCID 68992474 | — |
反応手順
To 4-fluoro-2-methoxybenzoic acid (0.96 g) was added concentrated sulfuric acid (6 mL) under ice-cooling, and the mixture was stirred for 15 minutes. To the mixture was added concentrated nitric acid (0.6 mL) under ice-cooling, and the mixture was stirred at the same temperature for 1 hour. To the reaction mixture was added ice, and the resulting mixture was stirred at room temperature for 10 minutes. The mixture was extracted with ethyl acetate. The extract was washed with water twice and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. To the residue was added a mixed solvent (n-hexane/ethyl acetate=2/1), and the insoluble material was collected by filtration, and dried under reduced pressure to give the title compound (0.78 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09040693B2 |
|---|
| 出典データセット | uspto-grants-2015_05 |
|---|
| ORD ID | ord-520ee4d53083427b9c3bfb6627d11da9 |
|---|
| 出典メモ | uspto-grants-2015_05 |
|---|