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 3-(4-tert-butylphenylsulfonamido)thiophene-2-carboxylate | HCID 8015643 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 3-(4-tert-butyl-n-methylphenylsulfonamido)thiophene-2-carboxylate | HCID 59180428 | 83.6% |
反応手順
To a solution of 55 (0.15 g; 0.42 mmol) in N,N-dimethylformamide (2 mL) at room temperature was added potassium carbonate (0.282 g; 2.12 mmol) followed by iodomethane (0.053 mL; 0.85 mmol). The reaction mixture was heated at 65° C. for 12 hours, cooled to room temperature, diluted with aqueous hydrochloric acid (50 mL; 2M) and extracted with dichloromethane (3×25 mL). The combined organic extracts were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to yield a crude residue that was purified by chromatography on silica gel eluting with a 0 to 10% ethyl acetate/hexanes gradient to give the title product (0.129 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08178699B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-111159a13811473b8c548de7de1a6a4a |
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| 出典メモ | uspto-grants-2012_05 |
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