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Ammonium Hydroxide → 4-Methyl-2-nitrobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 4-Methyl-2-nitrobenzoic acid | HCID 255027 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Methyl-2-nitrobenzamide | HCID 13244369 | 160.9% |
反応手順
To a solution of 4-methyl-2-nitrobenzoic acid (1.0 g, 5.52 mmol) in toluene (5 mL) was added oxalyl chloride (1.04 g, 8.28 mmol) at 0° C. and the reaction mixture was stirred at rt for 2 h. Then the reaction mixture was concentrated and the concentrate was dissolved in THF (5 mL). Then NH4OH (1.93 g, 55.20 mmol) was added to the solution at 0-5° C. and the reaction mixture was stirred at rt for 4 h before it was quenched with water and was extracted with EtOAc. The organic layer was washed with brine, separated, dried, filtered and concentrated to afford 1.6 g of the desired product. 1H NMR (300 MHz, DMSO-d6): δ 8.08 (br s, 1H), 7.79 (s, 1H), 7.62 (br s, 1H), 7.57-7.50 (m, 2H), 2.41 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09006257B2 |
| 出典データセット | uspto-grants-2015_04 |
| ORD ID | ord-356b990816db44e093bb45f3d85d6216 |
| 出典メモ | uspto-grants-2015_04 |