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3-Aminobenzoic Acid → HCID 178479313、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Aminobenzoic Acid | HCID 7419 | — |
| 反応物 | Benzenecarboximidic acid, ethyl ester, hydrochloride (1:1) | HCID 79249 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 178479313 | HCID 178479313 | 15.8% |
反応手順
To ethyl benzimidate hydrochloride (3 g, 0.016 mole)(Fluka) and (2.1 g, 0.016 mole) diisopropylethylamine in H2O (15 ml) and dioxane (15 ml) was added 3-aminobenzoic acid (2.22 g, 0.016 mole) (Aldrich). The reaction mixture was stirred at room temperature for 4 days. The resulting precipitate was filtered, washed with dioxane/H2O and dried. The precipitate was slurried in H2O and acidified with concentrated HCl. The solvent was removed under vacuum and the residue was slurried in ether. The ether was decanted off and the residue dried under vacuum to yield N-(3-carboxyphenyl)benzamidine hydrochloride (700 mg) as a white solid. MS and NMR were consistent with the desired structure.
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-20ecb093fda34faba4686369b6b1f19d |
| 出典メモ | uspto-grants-2000_02 |