関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-(4-Chlorobenzyl)piperidine | HCID 3732780 | — |
| 反応物 | 3-Butynyltosylate | HCID 18428004 | — |
| 生成物 | 1-(3-Butynyl)-4-(4-chlorophenyl)piperidine | HCID 18427968 | — |
反応手順
A suspension of NaHCO3 (4 g) and 4-[(4-chlorophenyl)methyl]piperidine (18 mmol) in dimethylformamide (DMF) (25 mL) is stirred under a N2 atm at 0° C., and treated dropwise with 3-butynyltosylate (20 mmol) as a solution in DMF (50 mL). The reaction mixture is heated at 80° C. and stirred an additional 18 hours. After cooling the reaction mixture is stirred vigorously with the addition of water (200 mL), and then extracted with ethyl acetate. The organic layer is dried over magnesium sulfate, filtered and evaporated. The residue is purified by silica gel column chromatography (100:1 CH2Cl2 :MeOH) to give 1-(3-butynyl)-4-(4-chlorophenyl)piperidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06130234 |
|---|
| 出典データセット | uspto-grants-2000_10 |
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| ORD ID | ord-b4438eb1509d411faa60c37bf1570671 |
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| 出典メモ | uspto-grants-2000_10 |
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