関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Ethynyloxolane | HCID 10034582 | — |
| 反応物 | 1-Benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene | HCID 22504376 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-(2-Tetrahydrofuranyl)-5-methanesulfonyl-1-benzenesulfonylindole | HCID 22504449 | 91.8% |
反応手順
To a solution of 1-benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene (256 mg) in 1,4-dioxane (6 ml), 2-ethynyltetrahydrofuran (169 mg), bistriphenylphosphine palladium dichloride (21 mg), cuprous iodide (11 mg) and triethylamine (89 mg) were added successively and the mixture was stirred in a sealed tube at 60° C. for 3 hours. After cooling, the reaction solution was poured into water, extracted with dichloromethane, 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=1:1) to obtain 218 mg of the desired product in a white amorphous form.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06673797B1 |
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| 出典データセット | uspto-grants-2004_01 |
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| ORD ID | ord-69ea4f2f131c4410be81dd751da3a87c |
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| 出典メモ | uspto-grants-2004_01 |
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