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Sodium Carbonate → 4-Piperidinol, 1-[2-[bis(4-fluorophenyl)methoxy]ethyl]-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Piperidin-4-ol | HCID 79341 | — |
| 反応物 | 1-[Bis(4-fluorophenyl)methoxy]-2-chloroethane | HCID 10779302 | — |
| 触媒 | Sodium Iodide | HCID 5238 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | 4-Piperidinol, 1-[2-[bis(4-fluorophenyl)methoxy]ethyl]- | HCID 9974982 | 66.4% |
反応手順
14.1 g of 1-bis(4-fluorophenyl)methoxy-2-chloroethane, 10.1 g of 4-hydroxypiperidine, 12 g of sodium carbonate and 0.2 g of sodium iodide were added to 200 ml of methyl isobutyl ketone, and the mixture was heated under reflux for 4 hours. At the end of this time, it was filtered, and the solvent was removed by distillation under reduced pressure. The resulting residue was purified by silica gel column chromatography. Elution with a 10:1 by volume mixture of ethanol and methylene chloride afforded 11.5 g (yield 66%) of the title compound as a pale yellow oily substance. p Infrared Absorption Spectrum (CHCl3), νmax cm-1 : 2920, 1600, 1505.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05294623 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-d698ffa795584a53a9f2a46741837185 |
| 出典メモ | uspto-grants-1994_03 |