関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl vinyl ketone | HCID 6570 | — |
| 反応物 | 4-(4-Chlorobenzyl)piperidine | HCID 3732780 | — |
| 触媒 | Water | HCID 962 | — |
| 生成物 | 4-(4-Chlorobenzyl)-1-(3-hydroxybutyl)piperidine hydrochloride | HCID 22004646 | 90% |
反応手順
2[1-(4-(4-chlorobenzyl)piperidin)]ethyl methyl ketone. To a solution of 4-(4-chlorobenzyl)piperidine (1.0 g, 4.78 mmol) in methyl vinyl ketone (1.0 ml) was added H2O (1 drop) and the resulting solution stirred at 110° C. for 2 h. The crude mixture was purified by filtration on silica gel using CH2Cl2/MeOH as eluant to afford the title compound (1.20 g, 90%) as a pale yellow oil: 1H NMR (CDCl3) 1.35-1.55 (m, 5H), 1.63 (d, J=12.3, 2H), 2.055 (t, J=9.6, 2H), 2.154: (s, 2H), 2.40 (d, J=6.3, 2H), 2.748 (s, 2H), 2.972 (d, J=11.4, 2H), 7.034 (d, J=8.1, 2H), 7.218 (d, J=8.1, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06218404B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-9e1ac1c482e84786947017d2d489ea41 |
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| 出典メモ | uspto-grants-2001_04 |
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