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Hydrochloric Acid → 1-Benzoylpiperidine-4-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Piperidinecarboxylic acid | HCID 3773 | — |
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Benzoylpiperidine-4-carboxylic acid | HCID 78935 | 44.3% |
反応手順
To a solution of 10 g of isonipecotic acid in 100 mL of water was added 31 mL of 5 N NaOH at 0° C. The reaction was warmed to room temperature and stirred for 0.5 h. The reaction was again cooled to 0° C. and 11.97 g of benzoyl chloride was added. The reaction was then warmed to room temperature and stirred for 1.5 h. Concentrated HCl was then added until a precipitate formed. The mixture was extracted with 3×150 mL of ethyl acetate and the combined organic layers were dried over magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was dissolved in methylene chloride. Ether was then slowly added to precipitate the product which was filtered to give 8 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06358979B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-fbe54d05da7f4ef39586a033f1f63d51 |
| 出典メモ | uspto-grants-2002_03 |