化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 178514389、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Aminobenzoic Acid | HCID 7419 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3,5-Dimethyl-1H-pyrazole-1-carboxamidine mononitrate | HCID 198186 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 178514389 | HCID 178514389 | 63.5% |
反応手順
A solution of 3-aminobenzoic acid (41.1 g) in dioxane (300 ml) was treated with 3,5-dimethyl(pyrazole-1-carboxamidine) HNO3 (100 g), DIEA (90 ml) and H2O (100 ml). The reaction was refluxed for 3 hours and stirred overnight at room temperature. The solid was filtered and washed with dioxane (150 ml) and 1:1 dioxane:H2O (250 ml). The solid was then suspended in diethyl ether (400 ml) and CH3CN (100 ml) and treated with 4N HCl/dioxane (100 ml) and 20% HCl (1 ml). After 48 hours, the reaction was filtered and dried to give 3-[(aminoiminomethyl)amino]benzoic acid (34.1 g) as a lavender solid. MS was consistent with the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06028223 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-37fed4d33f5740278aa9050f5b1c5bd0 |
| 出典メモ | uspto-grants-2000_02 |