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HRID 609597作成日:2026年10月26日
N-[(1-benzyl-4-piperidyl)methyl] 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide oxalate salt → N-(4-Piperidylmethyl) 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide
https://huagongshe.com/reaction/609597
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | N-[(1-benzyl-4-piperidyl)methyl] 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide oxalate salt | HCID 19599416 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-(4-Piperidylmethyl) 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide | HCID 9839803 | 105.4% |
反応手順
A stirred suspension of N-[(1-benzyl-4-piperidyl)methyl] 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide oxalate salt (E20, 2.25 g, 0.0046 mole) in ethanol (100 ml) and glacial acetic acid (4 ml) was hydrogenated over 10% Pd-C (0.8 g) at atmospheric pressure and 45° C. for 18 h. The mixture was filtered and the filtrate concentrated in vacuo. The majority of the product was in the solid which had been filtered off. This material was shaken with concentrated potassium carbonate solution (50 ml) and chloroform (50 ml) together with the residue from the filtrate. The mixture was filtered, the chloroform layer separated and dried (Na2SO4), then concentrated in vacuo to afford the title compound as a white solid (1.52 g, 100%). This was recrystallised from chlorofornm/60-80 petrol mp 139-141° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05998409 |
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| 出典データセット | uspto-grants-1999_12 |
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| ORD ID | ord-ed20c27d31994e61b67e037e60ae3473 |
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| 出典メモ | uspto-grants-1999_12 |
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