関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 6-Bromo-7,8,9,10-tetrahydro-2,3-dimethoxy-8-methyl-pyrido[4,3-f]quinoxaline | HCID 10065700 | — |
| 反応物 | CID 53628100 | HCID 178418400 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 7,8,9,10-Tetrahydro-2,3-dimethoxy-6,8-dimethyl-pyrido[4,3-f]quinoxaline | HCID 10378594 | 48% |
反応手順
A solution of the product from Example 100 (0.50 g, 1.48 mol) in 20 mL of tetrahydrofuran was cooled to −78° C. and treated dropwise with sec-BuLi (1.7 mL, 1.17 M in cyclohexane). The resulting green-black solution was stirred at −78° C. for 30 minutes. The reaction mixture was treated with MeI (123 μL, 2.00 mmol) and the resulting solution stirred at −78° C. for 30 minutes. The reaction mixture was warmed to room temperature and quenched with saturated aqueous NH4Cl solution (2.0 mL). The reaction mixture was extracted with CHCl3 (4×20 mL) and the combined organic extracts were dried and concentrated. The residue was broken up in heptane and collected by suction filtration to give the title compound as a orange solid (0.196 g, 48% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06703391B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-02eb257edce74edda79b5c69318ebc6e |
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| 出典メモ | uspto-grants-2004_03 |
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