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Sodium Carbonate → Ethyl 8-Amino-3,6-dimethylimidazo[1,2-a]pyridin-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 5-Methylpyridine-2,3-diamine | HCID 10701825 | — |
| 反応物 | Ethyl 3-bromo-2-oxobutanoate | HCID 11117285 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 8-Amino-3,6-dimethylimidazo[1,2-a]pyridin-2-carboxylate | HCID 22997462 | 30% |
反応手順
A solution of 2,3-diamino-5-methyl-pyridine (2.3 g, 19 mmol) and 3-bromo-2-oxo-butyric acid ethyl ester (4.3 g, 21 mmol) in ethanol (25 ml) was refluxed for 20 h. Sodium carbonate (2.6 g, 25 mmol) was added and the mixture was filtrated and the solids were washed with ethanol. The filtrate and washings were combined and evaporated under reduced pressure. The residue was dissolved in methylene chloride, washed twice with a sodium carbonate solution and twice with water. The organic layer was separated dried (Na2SO4) and evaporated under reduced pressure. Purification of the residue by column chromatography on silica gel using methylene chloride:methanol (9:1) as eluent gave 1.3 g (30%) of the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06613775B1 |
| 出典データセット | uspto-grants-2003_09 |
| ORD ID | ord-9ac846ac82824d0380d10e1389d08ed7 |
| 出典メモ | uspto-grants-2003_09 |