関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | 1H-Imidazole-4,5-dicarboxylic acid, 4,5-dimethyl ester | HCID 76810 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1H-Imidazo[4,5-d]pyridazine-4,7-diol | HCID 222923 | 60% |
反応手順
1H-Imidazole-4,5-dicarboxylic acid dimethyl ester (592 mg, 3.21 mmol) is combined with hydrazine (600 mg, 18.8 mmol) and MeOH (10 mL). The reaction mixture is heated to 115° C. for 30 min. Cool and filter off the resulting precipitate. Wash with additional water. Combine the precipitate with hydrazine (1.38 mL) and reflux for 4 h. Pour the reaction mixture into ice water and adjust the to pH 2 with HCl (12 N). The new precipitate is isolated by filtration to afford the title product (293 mg, 60%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536168B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-6c20aee492c64863989a5efab42e3ca4 |
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| 出典メモ | uspto-grants-2013_09 |
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