関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phthalazine | HCID 9207 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 5-Nitrophthalazine | HCID 11105874 | 47% |
反応手順
The 5-nitrophthalazine of formula (Y) was prepared according to prior art literature (Patrick, J.; Ragunathan, R., J. Chem. Soc. Perkin Trans. I, 1993, 211). A reaction vessel charged with phthalazine (the compound of formula (X), 4.0 g, 30 mmol) in conc. 96% sulfuric acid (30 mL) was further charged with potassium nitrate (14.6 g, 144 mmol) in small portions. Once the addition was complete, the solution was heated to 110° C. overnight. The mixture was then poured over ice and neutralized with sodium hydroxide solution resulting in the formation of a precipitate. The solid was isolated by filtration to yield 2.5 g (47%) of 5-nitrophthalazine of formula (Y) which was used in the following reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07875728B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-fc09f74475e64d0c84b7c92670b6aa1d |
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| 出典メモ | uspto-grants-2011_01 |
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