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HRID 1182898作成日:2026年10月27日

Water → 1-[2-(2-Hydroxy-phenyl)-2-oxo-ethyl]-3-methyl-7-(3-methyl-2-buten-1-yl)-8-[3-(tert.-butyloxycarbonylamino)-piperidin-1-yl]-xanthine

https://huagongshe.com/reaction/1182898

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Sodium CarbonateHCID 10340—
反応物3-(Boc-amino)piperidineHCID 4233041—
反応物1-[2-(2-Hydroxy-phenyl)-2-oxo-ethyl]-3-methyl-7-(3-methyl-2-buten-1-yl)-8-chloro-xanthineHCID 57514534—
溶媒Dimethyl SulfoxideHCID 679—
生成物1-[2-(2-Hydroxy-phenyl)-2-oxo-ethyl]-3-methyl-7-(3-methyl-2-buten-1-yl)-8-[3-(tert.-butyloxycarbonylamino)-piperidin-1-yl]-xanthineHCID 66723736—

反応条件

温度60 °C

反応手順

1.30 g of 3-tert.-butyloxycarbonylamino-piperidine are added to a mixture of 2.51 g of 1-[2-(2-hydroxy-phenyl)-2-oxo-ethyl]-3-methyl-7-(3-methyl-2-buten-1-yl)-8-chloro-xanthine and 880 mg of sodium carbonate in 8 ml of dimethylsulphoxide. The reaction mixture is stirred for 18 hours at 60° C. For working up it is combined with water and the precipitate formed is suction filtered. The solid crude product is dissolved in ethyl acetate, the solution is dried over magnesium sulphate and evaporated down. The flask residue is chromatographed through a silica gel column with cyclohexane/ethyl acetate (10:1 to 1:1) as eluant.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08664232B2
出典データセットuspto-grants-2014_03
ORD IDord-54926846360c426097bf59550516f7fb
出典メモuspto-grants-2014_03