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Hydrochloric Acid → 2-[[2-(4-Carboxyphenyl)ethyl]amino]-5-chloro-3-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,5-Dichloro-3-nitrobenzoic acid | HCID 6951 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(2-Aminoethyl)benzoic acid | HCID 506066 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-[[2-(4-Carboxyphenyl)ethyl]amino]-5-chloro-3-nitrobenzoic acid | HCID 54298812 | 57.5% |
反応手順
A mixture of 2,5-dichloro-3-nitrobenzoic acid (23.6 g, 100 mmol), powdered potassium carbonate (41.1 g, 300 mmol), and 4-(aminoethyl)benzoic acid (60.04 g, 400 mmol) in 250 ml of methanol was refluxed under argon for 18 hours. The reaction mixture was poured into 650 ml of 10% aqueous hydrochloric acid solution. The solid was collected and triturated with ethyl acetate. The ethyl acetate extract was decanted, dried with magnesium sulfate and concentrated in vacuo to give 20.15 g (57.5%) of the title compound; mp 255°-257° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05294631 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-b6c7993ebd9f4a05b43ed91b3538a110 |
| 出典メモ | uspto-grants-1994_03 |