参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 反应物 | 4-(4-Phenoxyphenyl)-1,2,3,6-tetrahydropyridine | HCID 22599989 | — |
| 催化剂 | HCID 178418390 | HCID 178418390 | — |
| 溶剂 | 醋酸 | HCID 176 | — |
| 产物 | 4-[(4-苯酚基)苯基]哌啶 | HCID 11075984 | 66% |
反应步骤
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%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US05723475 |
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| 来源数据集 | uspto-grants-1998_03 |
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| ORD ID | ord-33d9f641c6034e9a99040843b1b7b174 |
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| 来源说明 | uspto-grants-1998_03 |
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