関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4-Bromo-2-methoxy-6-nitroaniline | HCID 50879056 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | N-(4-bromo-2-methoxy-6-nitrophenyl)acetamide | HCID 53491145 | 75% |
反応手順
To a solution of 4-bromo-2-methoxy-6-nitrobenzenamine (27.85 g) in HOAc (150 mL) and Ac2O (17 mL) was added conc. H2SO4 at 70° C. and the mixture was stirred at 70° C. for 30 min and kept at rt overnight. The formed precipitate was collected by filtration and washed with hexane to afford the desired product as a light yellow solid (24.45 g, 75%). 1H NMR (300 MHz, DMSO-d6) δ ppm 2.01 (s, 3H), 3.92 (s, 3H), 7.61 (d, 1H, J=1.8 Hz), 7.65 (d, 1H, J=1.8 Hz), 9.91 (s, 1H); LC-MS: m/e=289 [M+1]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08541411B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-05be219954e84e998756ab0b54497e7c |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|
