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HRID 539900作成日:2026年10月27日

Sodium methanethiolate → 2-Chloro-4-(methylthio)pyrimidine

https://huagongshe.com/reaction/539900

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium methanethiolateHCID 4378561—
反応物2,4-Dichloro-5-ethylpyrimidineHCID 10012458—
溶媒TetrahydrofuranHCID 8028—
溶媒Ethyl AcetateHCID 8857—
生成物2-Chloro-4-(methylthio)pyrimidineHCID 1642714853.6%

反応手順

To a solution of ethyl 2,4-dichloropyrimidine (20.0 g, 0.13 mol) in 150 mL of anhydrous tetrahydrofurane was added sodium thiomethoxide (49.30 mL, 0.15 mol) at −10° C. The reaction mixture was allowed to warm up to room temperature and then stirred for 5 hours with monitoring a reaction with LC-MS or thin layer chromatography (TLC). The reaction mixture was diluted with ethyl acetate and washed with brine (×2). The collected organic layer was dried over anhydrous sodium sulfate and then concentrated in vacuo. The resulting solid was slurrified with diethyl ether and then collected by filtration to afford the desired intermediate 10 as a white solid (11.2 g, 52%)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08871778B2
出典データセットuspto-grants-2014_10
ORD IDord-4f1103dca1964454aec85ad23af160f0
出典メモuspto-grants-2014_10