関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Nitrobenzoic Acid | HCID 6108 | — |
| 反応物 | 2-Methoxyaniline | HCID 7000 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-methoxyphenyl)-4-nitrobenzamide | HCID 774513 | 87.5% |
反応手順
With cooling in an ice bath, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC.HCl) (630 mg, 3.29 mmol) was added to 15 ml of methylene chloride solution containing o-anisidine (368 mg, 2.99 mmol) and 4-nitrobenzoic acid (500 mg, 2.99 mmol). After 1 hour of stirring at the same temperature, the reaction mixture was roughly adjusted to pH 8 with saturated sodium bicarbonate aqueous solution, extracted with methylene chloride and then washed with water and saturated brine in that order. After drying on anhydrous magnesium sulfate, the solvent was removed by evaporation, and the resulting solid material was purified by silica gel column chromatography (methylene chloride) to obtain 712 mg (87.4%) of the title compound in the form of yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728835 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-c4ba4a81e15b4995a5093c01878efc4c |
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| 出典メモ | uspto-grants-1998_03 |
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