関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Chloro-N-methyl[3,4′-bipyridin]-2′-amine | HCID 16108983 | — |
| 反応物 | HCID 178507770 | HCID 178507770 | — |
| 生成物 | HCID 57756228 | HCID 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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09242961B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-6486f8804bb04e5694c700f090d74a35 |
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| 出典メモ | uspto-grants-2016_01 |
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