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HRID 593948作成日:2026年10月25日

Dimethyl Sulfoxide → HCID 57756228、化合物

https://huagongshe.com/reaction/593948

反応式

関与物質

役割名称HCID仕込み量
反応物Dimethyl SulfoxideHCID 679—
反応物Cesium carbonateHCID 10796—
反応物2-Chloro-N-methyl[3,4′-bipyridin]-2′-amineHCID 16108983—
反応物HCID 178507770HCID 178507770—
生成物HCID 57756228HCID 57756228—

反応手順

In a microwave vial, 5-aminopyridin-2-ol (125 mg, 1.14 mmol) was dissolved in DMSO (0.910 mL, 0.228 mmol) and cesium carbonate (445 mg, 1.37 mmol) was added. The vial was capped with a septum and the reaction was stirred at RT for 25 minutes until a paste was formed. Then 4-(2-chloropyridin-3-yl)-N-methylpyridin-2-amine (50 mg, 0.23 mmol) was added and the vial was sealed and heated to 180° C. in Personal Chemistry Microwave for 15 min. The mixture was extracted with EtOAc, organic layers were washed with brine, dried over MgSO4, filtered, and concentrated. The product was purified by column chromatography on silica gel using 60:40 DCM:(90:10:1 DCM:MeOH:NH4OH to flush out top spots, then 50:50 DCM:(90:10:1 DCM:MeOH:NH4OH) to collect the product. Green solid, 4-(2-(5-aminopyridin-2-yloxy)pyridin-3-yl)-N-methylpyridin-2-amine was obtained. MS m/z=294 [M+1]+. Calcd for C16H15N5O: 293.13.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09242961B2
出典データセットuspto-grants-2016_01
ORD IDord-6486f8804bb04e5694c700f090d74a35
出典メモuspto-grants-2016_01