関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Ethyl bromopyruvate | HCID 66144 | — |
| 反応物 | N5,N5-Dimethylpyridine-2,5-diamine | HCID 5743468 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | Ethyl 6-dimethylaminoimidazo[1,2-a]pyridine-2-carboxylate | HCID 44124134 | — |
反応手順
To a suspension of 0.2 g of 5-dimethylaminopyridine-2-amine in 3 mL of DME are added 215 μL of ethyl bromopyruvate. The reaction mixture is stirred at 20° C. for 16 hours and then, after addition of 3 mL of ethanol, for 16 hours at reflux, and finally concentrated under reduced pressure. The residue is filtered on a cartridge of 15 g of silica, eluting with a mixture of dichloromethane and methanol (98/2). The fractions containing the expected product are combined and washed with saturated sodium bicarbonate solution. The organic phase is dried and concentrated to dryness under reduced pressure to give 76 mg of ethyl 6-dimethylaminoimidazo[1,2-a]pyridine-2-carboxylate in the form of a green oil, which is used without further purification in the rest of the synthesis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07902219B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-b32fd19204cd4b839ca6f5a53c41e8d4 |
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| 出典メモ | uspto-grants-2011_03 |
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