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 | 1-Chlorophthalazine | HCID 160793 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Hydralazine | HCID 3637 | 99% |
反応手順
A 2 L, 3-necked, round-bottomed flask fitted with a temperature probe and condenser, and was charged 375 mL of hydrazine hydrate; the solution was then cooled to 0 to 5° C. About 75 g of 1-chlorophthalazine salt was added in portions at a rate to maintain the solution temperature at 0 to 5° C. After addition, the solution was stirred at 20 to 25° C. for about 24 hrs. The reaction mixture was then cooled to 0 to 5° C. and 150 mL of methanol was added, the solution stirred for 3 hrs, and the resulting solid material was filtered, washed with 150 mL of cold methanol, and dried under vacuum at 35° C. Yield 99%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07531653B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-35f0bfb01b28422585845fb955d5cc72 |
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| 出典メモ | uspto-grants-2009_05 |
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