関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | 2-Benzenesulfonylamino-3-iodo-5-methylthiopyridine | HCID 15486851 | — |
| 反応物 | 5-Ethoxycarbonyl-2-trimethylsilylethynylpyridine | HCID 22504397 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 6-(1-Benzenesulfonyl-5-methylthio-1h-pyrrolo[2,3-b]pyridin-2-yl)nicotinic acid ethyl ester | HCID 68444739 | 98.5% |
反応手順
To a solution of 2-benzenesulfonylamino-5-methylthio-3-iodo-pyridine (100 mg) in 1,4-dioxane (2.5 ml), 5-ethoxycarbonyl-2-trimethylsilylethynylpyridine (185 mg), bistriphenylphosphine palladium dichloride (9 mg), cuprous iodide (5 mg) and potassium acetate (37 mg) were added successively and the mixture was stirred in a sealed tube at 100° C. for 15 hours. After cooling, the reaction solution was poured into water, extracted with ethyl acetate, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was separated using silica gel preparative thin-layer chromatography (hexane:ethyl acetate=2:1) to obtain 110 mg of the desired product as an orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06875770B2 |
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| 出典データセット | uspto-grants-2005_04 |
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| ORD ID | ord-0f1fd7e7c0f54fbc91234c3ff00dc5b1 |
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| 出典メモ | uspto-grants-2005_04 |
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