化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Iodide → 4'-Tert-butyl-6-[4-(alpha-hydroxy-alpha-phenylbenzyl)piperidino]caprophenone hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Azacyclonol | HCID 15723 | — |
| 反応物 | Potassium Bicarbonate | HCID 516893 | — |
| 反応物 | 4'-Tert-butyl-6-chlorocaprophenone | HCID 21552993 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4'-Tert-butyl-6-[4-(alpha-hydroxy-alpha-phenylbenzyl)piperidino]caprophenone hydrochloride | HCID 21552957 | — |
反応手順
A mixture of 22.4 g (0.08 mole) of α,α-diphenyl-4-piperidinemethanol, 23.8 g (0.09 mole) of 4'-tert-butyl-6-chlorocaprophenone, 20 g (0.2 mole) of potassium bicarbonate, 0.1 g of potassium iodide in 300 ml of toluene and 45 ml of water is stirred on a steam bath for about 96 hours after which the organic layer is separated and combined with toluene extracts of the aqueous layer. The combined organic material is washed with water and saturated sodium chloride solution, dried over magnesium sulfate, and filtered. The filtrate is diluted with ether and made acidic with ethereal HCl. The resulting precipitate is recrystallized from methanol-butanone to give 4'-tert-butyl-6-[4-(α-hydroxy-α-phenylbenzyl)piperidino]caprophenone hydrochloride.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03946022 |
| 出典データセット | uspto-grants-1976_03 |
| ORD ID | ord-0999aa34735c40f8adce64a580f06ea6 |
| 出典メモ | uspto-grants-1976_03 |