関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 1(2H)-Phthalazinone | HCID 8394 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-Chlorophthalazine hydrochloride | HCID 22386464 | — |
反応手順
A suspension of 50 g (342 mmol) phthalazone, 1370 ml acetonitrile, 66 ml (0.72 mol) POCl3 and 85 ml 4 N HCl in dioxane is stirred for 8 h at 50° C. The resulting solution is cooled to RT, evaporated to a volume of about 0.8 l and diluted with 1.2 I DIPE. Filtration and washing with DIPE yield the title compound: FAB-MS (M+H)+=165/167.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07329660B2 |
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| 出典データセット | uspto-grants-2008_02 |
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| ORD ID | ord-2a2581d1ba764f06aa962befd0b91fe5 |
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| 出典メモ | uspto-grants-2008_02 |
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