関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(4-Nitrobenzyl)piperidine | HCID 783541 | — |
| 反応物 | Piperidin-1-ylmethyl-phenylamine | HCID 21974891 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178418702 | HCID 178418702 | — |
反応手順
1-(4-Nitro-benzyl)-piperidine (0.5052 gms.) is suspended in 25 mL of a 1:1 (v:v) solution of acetic acid and water. The suspension is then treated with 45 mL of an ˜10 wt. % solution of TiCl3 in 20–30 wt. % HCl, dropwise. Over the course of the addition a color change from colorless to purple to black ensues. The reaction mixture is immersed in a 60° C. oil bath overnight following the addition of TiCl3. The reaction mixture is then cooled to room temperature and made basic with the addition of a 10% aqueous solution of NaOH. The basic reaction mixture is extracted with chloroform, and the organic layer is dried over anhydrous sodium sulfate. Following evaporation of the solvent the organic layer yields 0.333 gms. of piperidin-1-ylmethyl-phenylamine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098236B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-1439421f0cf641689aef96f1a9448bf3 |
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| 出典メモ | uspto-grants-2006_08 |
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