関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Nitrophthalic anhydride | HCID 21631 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1,4-Phthalazinedione, 2,3-dihydro-5-nitro- | HCID 3525223 | 92% |
反応手順
A glass flask of the volume 1 l provided with an agitator, a thermometer, a condenser and a capillary was filled with 600 ml of icy acetic acid and 154.5 g (0.8 mole) of 3-nitrophthalic acid anhydride, thereafter it was heated to the temperature of 110° C. and gradually 44.1 g (0.88 mole) of hydrazine hydrate was added. Next the reaction mixture was kept at the state of boiling for 30 minutes thereafter it was cooled to the temperature of 80° C., the crystals of 5-nitro-2,3-dihydrophthalazine-1,4-dione were filtered, the sediment was washed on a filter with 50 ml of acetic acid and two times with 40 ml of distilled water. The total amount of 5-nitro-2,3-dihydrophthalazine-1,4-dione was 228.7 g, the yield was 92%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536171B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-9911b083cac04d16b4d8d7c9b4d66c81 |
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| 出典メモ | uspto-grants-2013_09 |
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