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Acetic Acid → 4-[Bis(4-fluorophenyl)methylene]-1-(phenylmethyl)piperidine
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 | Water | HCID 962 | — |
| 反応物 | alpha,alpha-Bis(4-fluorophenyl)-1-(phenylmethyl)-4-piperidinemethanol | HCID 13519964 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-[Bis(4-fluorophenyl)methylene]-1-(phenylmethyl)piperidine | HCID 13519965 | — |
反応手順
A mixture of 40 parts of α,α-bis(4-fluorophenyl)-1-(phenylmethyl)-4-piperidinemethanol, 120 parts of a hydrochloric acid solution and 50 parts of acetic acid was stirred and refluxed for 2 hours. The reaction mixture was cooled and water and methylbenzene were added: three layers were obtained. The two supernatant phases were separated and treated with ammonium hydroxide. The organic phase was separated, dried, filtered and evaporated. The residue was crystallized from 2,2'-oxybispropane, yielding 26 parts of 4-[bis(4-fluorophenyl)methylene]-1-(phenylmethyl)piperidine (intermediate 13).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04581171 |
| 出典データセット | uspto-grants-1986_04 |
| ORD ID | ord-92acec2014b74d78a7e76b34a69b970b |
| 出典メモ | uspto-grants-1986_04 |