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Hydrazine hydrate (1:1) → 4-Phenylpyridazine-3,6-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Phenylmaleic anhydride | HCID 99174 | — |
| 反応物 | Sodium Acetate Trihydrate | HCID 23665404 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-Phenylpyridazine-3,6-dione | HCID 18430681 | 33.9% |
反応手順
Phenylmaleic anhydride (20 g, 115 mmol), sodium acetate trihydrate (1875 g, 138 mmol), hydrazine monohydrate (6.68 ml, 133 mmol) and 40% aqueous acetic acid (400 ml) were heated at reflux for 15 h then allowed to cool. The reaction mixture was left to cool in the fridge for 1 h. The solid produced was filtered and washed with water and diethyl ether before drying in a vacuum oven at 40° C. to give the required product (7.26 g). 1H NMR (250 MHz, DMSO) δ 3.43 (2H, broad peak), 7.17 (1H, s), 7.44 (3H, m), 7.81 (2H, m); MS (ES+) m/e 189 [MH+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06297235B1 |
| 出典データセット | uspto-grants-2001_10 |
| ORD ID | ord-0b3c74bd81ff4dd9a780a64a0ba0942c |
| 出典メモ | uspto-grants-2001_10 |