化工社化工社 化学情報印刷レポート · 研究参考用
Methylamine → 4-(Methylamino)-3-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 4-Chloro-3-nitrobenzoic acid | HCID 7320 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(Methylamino)-3-nitrobenzoic acid | HCID 283475 | 86% |
反応手順
A mixture comprising 3-nitro-4-chlorobenzoic acid (1.3 g, 6.45 mmol), 10% methylamine and water (10 mL) in a sealed tube was heated at 100° C. for 11 hours, concentrated to 1 mL and then diluted with concentrated hydrochloric acid to give a yellow precipitate. The precipitate was isolated by filtration, washed with water and then diethyl ether and dried to provide 3-nitro-4-methylaminobenzoic acid (2.1 g, 86% yield); 1H-NMR (300 Mhz, CDCL3): 8.56 (d, 1H, J=2.1 Hz), 8.52 (q, 1H, J=8.6 Hz), 7.94 (dd, 1H, 9.3, 2.1 Hz), 7.00 (d, 1H, J=9.3 Hz), 2.97 (d, 3H, J=8.6 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06562854B2 |
| 出典データセット | uspto-grants-2003_05 |
| ORD ID | ord-4bb4c4734d4e4339b02bb02b62c8ba9b |
| 出典メモ | uspto-grants-2003_05 |