関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 5-Hydroxy-4-methoxy-2-nitrobenzoic acid | HCID 13915669 | — |
| 触媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | Methyl 5-hydroxy-4-methoxy-2-nitrobenzoate | HCID 53396387 | 45% |
反応手順
To a suspension of 5-hydroxy-4-methoxy-2-nitrobenzoic acid (8.0 g, 37.5 mmol) in methanol was added concentrated sulfuric acid (3 drops) and it was heated at 80° C. overnight. After solvent was removed under reduced pressure, to it was added water and EtOAc. The organic layer was washed with saturated NaHCO3 solution, dried over MgSO4, and concentrated under reduced pressure to afford methyl 5-hydroxy-4-methoxy-2-nitrobenzoate as a solid (3.86 g, 45%). 1H NMR (300 MHz, DMSO-d6) δ 10.96 (s, 1H), 7.63 (s, 1H), 7.08 (s, 1H), 3.91 (s, 3H), 3.81 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08969587B2 |
|---|
| 出典データセット | uspto-grants-2015_03 |
|---|
| ORD ID | ord-e494c87262b74edaa1abba2108201b9a |
|---|
| 出典メモ | uspto-grants-2015_03 |
|---|