関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-one | HCID 67328898 | — |
| 反応物 | HCID 178512500 | HCID 178512500 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 67327913 | HCID 67327913 | — |
| 生成物 | 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid methyl ester | HCID 67354675 | — |
反応手順
To a solution of 3-Dimethylaminomethylene-1-(2-methyl-5-nitro-phenyl)-piperidin-4-one (12.06 gm, 41.7 mmol)[as prepared in reference 1] in Ethanol (250 ml) were added N-(4-Chloro-phenyl)-guanidine (28.32 gm, 167 mmol) and sodium acetate (27.32 gm, 334 mmol) and solution was heated under reflux for 12 hours. After cooling to room temperature, the reaction mixture was diluted with water, extracted with ethyl acetate. The organic layer was washed with brine, dried [sodium sulfate] and concentrated under vacuum. The crude product obtained was further purified by silica gel chromatography using 5-10% Methanol/Chloroform as eluent to give pure desired product [11] i.e., (4-Chloro-phenyl)-[6-(2-methyl-5-nitro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-amine as yellow solid. (Yield: 2.50 gm, 15.2%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08962637B2 |
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| 出典データセット | uspto-grants-2015_02 |
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| ORD ID | ord-47ade73e82444c86a09c1581f508b7cf |
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| 出典メモ | uspto-grants-2015_02 |
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