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HRID 1853950作成日:2026年10月25日

Ethanol → HCID 67327913、化合物

https://huagongshe.com/reaction/1853950

反応式

関与物質

役割名称HCID仕込み量
反応物EthanolHCID 702—
反応物Sodium AcetateHCID 517045—
反応物3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-oneHCID 67328898—
反応物HCID 178512500HCID 178512500—
溶媒WaterHCID 962—
生成物HCID 67327913HCID 67327913—
生成物3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid methyl esterHCID 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

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-47ade73e82444c86a09c1581f508b7cf
出典メモuspto-grants-2015_02