関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl 4-chloro-3-nitrobenzoate | HCID 735797 | — |
| 反応物 | 1-[4-(3-Aminophenyl)piperazin-1-yl]ethan-1-one | HCID 11117539 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | Methyl 4-(3-(1-acetylpiperazin-4-yl)anilino)-3-nitrobenzoate | HCID 22741905 | 85% |
反応手順
To a solution of methyl 4-chloro-3-nitrobenzoate (2.0 g, 9.28 mmol) in anhydrous NMP (5 ml) was added 2d (2.03 g, 9.28 mmol) and triethylamine (1.3 ml, 9.28 mmol). The mixture was heated with stirring to 80° C. overnight. The cooled solution was poured into ice-water (50 ml) and the resulting mixture was extracted with ethyl acetate (3×10 ml). The combined organic extracts were washed with water, dried over sodium sulfate and evaporated to dryness. The residue was triturated with petroleum ether to yield methyl 4-(3-(1-acetylpiperazin-4-yl)anilino)-3-nitrobenzoate (3.14 g, 85%) as red crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06710044B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-d28c7b02f5b34d5cb4e0639f13bf4dc5 |
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| 出典メモ | uspto-grants-2004_03 |
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