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Sulfuric Acid → 1-Ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamide | HCID 59614586 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-Ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester | HCID 59614592 | — |
反応手順
1.4 ml of concentrated sulfuric acid is slowly added to a solution of 4.3 g of N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamide in 11 ml of methanol. After stirring 20 hours under reflux, the reaction mixture is allowed to cool down to room temperature and diluted with ice water. Sodium carbonate is added and the aqueous phase is extracted with ethyl acetate. The organic phase is dried over sodium sulfate, filtered and concentrated. Chromatography (dichloromethane+1% of ethanol) gave 3.2 g of 1-ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester as a solid, mp: 131-132° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08722578B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-5f7ea7b5e80f49749e3f42e2f9de96cb |
| 出典メモ | uspto-grants-2014_05 |