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
215 μl of ethyl bromopyruvate are added to a suspension of 0.2 g of 5-dimethylaminopyridine-2-amine in 3 ml of DME. The reaction mixture is stirred at 20° C. for 16 hours, 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 comprising 15 g of silica, elution being carried out with a mixture of dichloromethane and methanol (98/2). The fractions comprising the expected product are combined and washed with a saturated sodium bicarbonate solution. The organic phase is dried and concentrated to dryness under reduced pressure to give 76 mg of ethyl 6-dimethylamino-imidazo[1,2-a]pyridine-2-carboxylate in the form of a green oil used as is in the continuation of the synthesis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07704989B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-638aea446ecf4c4e9f905d5163c291dd |
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| 出典メモ | uspto-grants-2010_04 |
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