関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 1-(4-(4-Chlorophenyl)-4-hydroxypiperidin-1-yl)-4-(4-fluorophenyl)butane-1,4-dione | HCID 21559988 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(4-Chlorophenyl)-alpha-(4-fluorophenyl)-4-hydroxy-1-piperidinebutanol | HCID 119265 | — |
反応手順
To a mixture of 2.0 g of lithium aluminum hydride and 50 ml of tetrahydrofuran, was gradually added a solution of 5.0 g of 1-[β-(p-fluorobenzoyl)propionyl]-4-(p-chlorophenyl)-4-hydroxypiperidine in 40 ml of tetrahydrofuran. The mixture was stirred at room temperature for one hour, and at 60°to 65°C for 4 hours. Then 15 ml of cold water was added dropwise to the reaction mixture while the mixture was kept below 20°C in an ice bath. The precipitate was filtered off and the tetrahydrofuran was removed from the filtrate by distillation under reduced pressure. The residue was kept cooled for 2 hours and the solid matter was collected by filtration, washed with water, and dried to obtain 1-(p-fluorophenyl)-4-[4-(p-chlorophenyl)-4-hydroxypiperidino]-1 -butanol, melting at 128° - 130°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03936468 |
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| 出典データセット | uspto-grants-1976_02 |
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| ORD ID | ord-4eb8283397294fecad7c0920a9cb540b |
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| 出典メモ | uspto-grants-1976_02 |
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