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HRID 57659作成日:2026年10月23日

Water → 3-chloro-5-methyl-7-neopentyl-2-(4-(pyridin-4-yl)benzyl)-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione

https://huagongshe.com/ja/reaction/57659

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物HexachloroethaneHCID 6214—
反応物Lithium HexamethyldisilazideHCID 2733832—
反応物5-methyl-7-neopentyl-2-(4-(pyridin-4-yl)benzyl)-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dioneHCID 70097472—
溶媒DichloromethaneHCID 6344—
溶媒TetrahydrofuranHCID 8028—
生成物3-chloro-5-methyl-7-neopentyl-2-(4-(pyridin-4-yl)benzyl)-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dioneHCID 7009533092.1%

反応手順

5-methyl-7-neopentyl-2-(4-(pyridin-4-yl)benzyl)-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (500 mg, 1.24 mmol) and hexachloroethane (587 mg, 2.48 mmol) are dissolved in 8 mL of methylene chloride, and then 1.0 M LiHMDS (2.48 mL, 2.48 mmol) in THF is added dropwise. After the reaction mixture is stirred at room temperature for 10 min, 100 mL of deionized water is added, and then extracted with methylene chloride four times (30 mL×4). The combined organic phase is dried over anhydrous sodium sulfate. After filtration, the filtrate is evaporated to dryness to give 500 mg of crude product as brown solids, which is used in the next step without further purification. MS (ESI) m/z 438.2 [M+H]+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09434730B2
出典データセットuspto-grants-2016_09
ORD IDord-4e697967616d4cdf8d5d6ee1edca4796
出典メモuspto-grants-2016_09