関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Lithium hydride | HCID 62714 | — |
| 反応物 | ((4-Bromobutoxy)methyl)benzene | HCID 4422181 | — |
| 反応物 | 6-Methoxypyrido[2,3-B]pyrazin-3(4H)-one | HCID 66739803 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-[4-(Benzyloxy)butyl]-6-methoxypyrido[2,3-b]pyrazin-3(4H)-one | HCID 86724962 | 74% |
反応手順
In N,N-dimethylformamide (15 ml) was dissolved 6-Methoxypyrido[2,3-b]pyrazin-3(4H)-one (600 mg, 3.39 mmol). The solution was cooled in an ice bath, lithium hydride (purity 90%, 35.9 mg, 4.06 mmol) was then added thereto and the mixture was stirred at room temperature for 40 minutes. The reaction solution was cooled again in an ice bath, benzyl 4-bromobutyl ether (0.774 ml, 4.06 mmol) and sodium iodide (609 g, 4.06 mmol) were added and then the mixture was stirred overnight at room temperature. The reaction solution was diluted with ethyl acetate, washed sequentially with saturated sodium chloride solution (2×), water and saturated sodium chloride solution, dried over anhydrous magnesium sulfate and the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to yield 847 mg (74%) of the title compound in the form of a light yellow syrup.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08952010B2 |
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| 出典データセット | uspto-grants-2015_02 |
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| ORD ID | ord-931ceb9b3eb548a3971227665a622668 |
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| 出典メモ | uspto-grants-2015_02 |
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