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Sodium Hydroxide → 3-(4-Nitrophenyl)propanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Propenoic acid, 3-(4-nitrophenyl)- | HCID 70156 | — |
| 反応物 | hydroxylamine-O-sulfonic acid | HCID 76284 | — |
| 反応物 | Hydroxylamine, sulfate (1:1) | HCID 159255 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(4-Nitrophenyl)propanoic acid | HCID 85526 | — |
反応手順
A suspension of 4-nitrocinnamic acid (13.5 g, 70 mmol) in H2O (100 mL) was treated with hydroxylamine sulfate (18.5 g, 113 mmol) and hydroxylamine-o-sulfonic acid (43.5 g, 385 mmol) at 0° C. The pH was adjusted to 7.6 with 50% NaOH, and additional base was added as needed over the next 6 hours to maintain a pH of 7.6. The mixture was then filtered, and the filtrate was acidified to pH 2 with 2N H2SO4. The solids that formed were filtered, washed with H2O, and recrystallized from EtOH:H2O(30 mL: 150 mL) to give the title compound. 1H NMR (CDCl3) δ 2.71 (t, 2 H), 3.03 (t, 2 H), 7.34 (d, 2 H), 8.13 (d, 2 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05834506 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-7888d33e742b4c49ae52644e34b85d58 |
| 出典メモ | uspto-grants-1998_11 |