関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl 4-[(methylsulfonyl)amino]-1H-indole-6-carboxylate | HCID 21086208 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | methyl 4-[methyl(methylsulfonyl)amino]-1H-indole-6-carboxylate | HCID 21086207 | 69.2% |
反応手順
To a mixture of Methyl 4-[(methylsulfonyl)amino]-1H -indole-6-carboxylate (0.6 g) in THF (10 mL) was added potassium carbonate (0.309 g) and iodomethane (0.63 mL). The mixture was stirred at room temperature for 4 h then heated to 40° C. overnight. Iodomethane (0.3 mL) was added and the mixture heated an additional 3 h. The mixture was cooled to room temperature, partitioned between water and diethyl ether, dried over anhydrous sodium sulfate and concentrated. The residue was dissolved in ether and decolorizing carbon (2 g) was added and the mixture refluxed for 5 minutes then filtered through celite while hot. The ether was removed under reduced pressure to give 0.437 g of the title compound: MS (ESI+) for C12 H14 N2 O4 Si m/z 321.1 (M+K).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727997B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-2d4556d0f71c4fc99fbb2155315f3880 |
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| 出典メモ | uspto-grants-2010_06 |
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