関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 3-Bromo-2,5-furandione | HCID 80027 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Acetic acid--water (1/1) | HCID 21899381 | — |
| 生成物 | 4-Bromopyridazine-3,6-diol | HCID 254942 | 37% |
反応手順
A mixture of bromomaleic anhydride (50 g, 283 mmol) and sodium acetate (76.5 g, 562 mmol) in 40% acetic acid/water (750 ml) was treated with hydrazine monohydrate (16.5 ml, 339 mmol) at room temperature under nitrogen. The brown solution was stirred and heated at 100° C. for 18 hours. Upon cooling the mixture was poured into water (11) and extracted with ethyl acetate (6×500 ml). The combined extracts were dried (MgSO4), filtered and evaporated to afford the title compound (20 g, 37%) as an orange solid. 1H NMR (250 MHz, d6-DMSO) δ7.68 (1H, br s). MS (ES+) m/e 193 [MH]+, 191 [MH]+. This material was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06699859B1 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-8aca293d090446adaace60d29ff64fea |
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| 出典メモ | uspto-grants-2004_03 |
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