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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 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Benzoylpiperidine-4-carboxylic acid | HCID 78935 | 95% |
反応手順
To an ice cold solution of isonipecotic acid (90 g, 0.697 mol) and potassium carbonate (81 g, 1.31 mol) in water (1.3 liter) was added dropwise benzoyl chloride (81 ml, 0.697 mol) over a period of about an hour at about 5° C. The mixture was stirred at room temperature overnight. The reaction mixture was acidified with 6N hydrochloric acid and extracted with dichloromethane. The organic layer was washed with water and then dried over magnesium sulfate and the solvent was evaporated in vacuo. Crystallization from isopropyl alcohol-diethyl ether to give the titled compound (154.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05948786 |
| 出典データセット | uspto-grants-1999_09 |
| ORD ID | ord-090031d131f24188b7adc55f41b6ba9b |
| 出典メモ | uspto-grants-1999_09 |