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HRID 10434作成日:2026年10月24日

3,4-dihydro-2H-pyran → 2,6-Dichloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purine

https://huagongshe.com/ja/reaction/10434

反応式

関与物質

役割名称HCID仕込み量
反応物3,4-dihydro-2H-pyranHCID 8080—
反応物Sodium BicarbonateHCID 516892—
反応物p-Toluenesulfonic acid monohydrateHCID 521998—
反応物2,6-dichloro-1H-purineHCID 178418875—
溶媒WaterHCID 962—
溶媒Ethyl AcetateHCID 8857—
生成物2,6-Dichloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purineHCID 270265—

反応条件

温度50 °C

反応手順

2,6-Dichloro-9H-purine (20 g, 0.11 mol) and 4-toluenesulphonic acid monohydrate (0.2 g) were dissolved in ethyl acetate (300 ml), the mixture heated to 50° C. and a solution of 3,4-dihydro-2H-pyran (12.6 ml, 0.14 mol) in ethyl acetate (50 ml) added slowly over 30 minutes. The reaction mixture was cooled to room temperature, water (100 ml) added and the pH of the solution adjusted to 7 by addition of a saturated aqueous solution of sodium hydrogen carbonate. The organic layer was separated, washed sequentially with water and brine, dried over anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure. The residue was azeotroped with pentane (×2) to afford the title compound as a slightly impure white solid (30.9 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07094769B2
出典データセットuspto-grants-2006_08
ORD IDord-69e4a8157db7424a83d31d8e7356ee4a
出典メモuspto-grants-2006_08