関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 4-chloro-3-nitrobenzoate | HCID 1268247 | — |
| 反応物 | 3-(1-Methyl-3-piperidinyl)aniline | HCID 22741929 | — |
| 生成物 | Ethyl 4-(3-(1-methylpiperidin-3-yl)phenylamino)-3-nitrobenzoate | HCID 22741906 | 98% |
反応手順
A mixture of 1c (5.7 g, 25 mmol), 2j (3.8 g, 20 mmol) and potassium carbonate (3.45 g, 25 mmol) was heated to 70° C. under a stream of nitrogen. The resulting melt was stirred at 70° C. overnight. The reaction mixture was partitioned between water and ethyl acetate and the organic phase was extracted with diluted hydrochloric acid (4M). The aqueous phase was rendered alkaline by addition of aqueous sodium hydroxide (4M) and extracted with ethyl acetate. The organic phase was dried over sodium sulfate and the solvent was removed under reduced pressure to leave ethyl 4-(3-(1-methylpiperidin-3-yl)phenylamino)-3-nitrobenzoate (7.5 g, 98%) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06218547B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-1d471ddf64eb42a2b9b033a10de4e4a2 |
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| 出典メモ | uspto-grants-2001_04 |
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