関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 4-(4-Phenoxyphenyl)-1,2,3,6-tetrahydropyridine | HCID 22599989 | — |
| 触媒 | HCID 178418390 | HCID 178418390 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-(4-Phenoxyphenyl)piperidine | HCID 11075984 | 66% |
反応手順
To a 100 ml methanol solution of 3.51 g of the compound (3) synthesized in Reference Example 3 were added 200 mg of palladium carbon and 1 ml of acetic acid for hydrogenation at atmospheric pressure and room temperature. After the end of the reaction, the insolubles were filtered off and the filtrate was concentrated under reduced pressure. The obtained residue was dissolved in methylene chloride, then adjusted by a 10% aqueous solution of sodium hydroxide to pH=9 to 10, then was shaken. The organic layer was dried, filtered, then concentrated under reduced pressure to obtain a residue which was then purified by silica gel column chromatography (methylene chloride:methanol=20:1!) to obtain the above-reference compound (4) in all amount of 2.32 g (yield of 66%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05723475 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-33d9f641c6034e9a99040843b1b7b174 |
|---|
| 出典メモ | uspto-grants-1998_03 |
|---|