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HRID 1853963作成日:2026年10月27日

Sodium Acetate → [6-(2-Methyl-5-nitro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-[4-(4-methyl-piperazin-1-yl)-phenyl]-amine

https://huagongshe.com/reaction/1853963

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium AcetateHCID 517045—
反応物3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-oneHCID 67328898—
反応物1-(4-(4-Methylpiperazin-1-yl)phenyl)guanidineHCID 178480747—
溶媒EthanolHCID 702—
溶媒WaterHCID 962—
生成物[6-(2-Methyl-5-nitro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-[4-(4-methyl-piperazin-1-yl)-phenyl]-amineHCID 67328470—

反応手順

To a solution of 3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)-piperidin-4-one (12.06 gm, 41.7 mmol)[as prepared in reference 1] in Ethanol (250 ml) were added N-[4-(4-Methyl-piperazin-1-yl)-phenyl]-guanidine (38.9 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 [47] i.e., [6-(2-Methyl-5-nitro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-[4-(4-methyl-piperazin-1-yl)-phenyl]-amine as yellow solid. (Yield: 3.65 gm, 19.0%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08962637B2
出典データセットuspto-grants-2015_02
ORD IDord-cb10d4bf5efb4a6e97b20e7f3b19818a
出典メモuspto-grants-2015_02