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HRID 581872作成日:2026年10月26日

Sodium Bicarbonate → 1-{[3,4-Di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl}-5-ethyl-6-phenylthio-2,4-pyrimidinedione

https://huagongshe.com/reaction/581872

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium BicarbonateHCID 516892—
反応物5-Ethyl-6-phenylthio-2,4-pyrimidinedioneHCID 10586637—
反応物[3,4-Di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl bromideHCID 54350482—
溶媒DimethylformamideHCID 6228—
生成物1-{[3,4-Di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl}-5-ethyl-6-phenylthio-2,4-pyrimidinedioneHCID 69976644—

反応手順

A mixture of 5-ethyl-6-phenylthio-2,4-pyrimidinedione (0.16 g, 0.66 mmol) and [3,4-di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl bromide (0.30 g, 0.66 mmol) in dimethylformamide (10 ml) were heated at 50° C. for overnight in the presence of sodium bicarbonate (66 mg, 0.79 mmol). After the concentration of dimethylformamide, 1-{[3,4-di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl}-5-ethyl-6-phenylthio-2,4-pyrimidinedione was obtained by the separation of the column chromatography. And then, this compound in THF (10 ml) was reacted with n-tetrabutylammonium fluoride at room temperature for 1 hr. After the concentration of THF, the residue was separated by column chromatography to give a desirable product (48 mg).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05922727
出典データセットuspto-grants-1999_07
ORD IDord-6f843d2e17714f198a85b4db06a30bbc
出典メモuspto-grants-1999_07