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 | Furan, 2-ethynyl- | HCID 140409 | — |
| 反応物 | 2-Benzenesulfonylamino-3-iodo-5-methylthiopyridine | HCID 15486851 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1H-Pyrrolo[2,3-b]pyridine, 2-(2-furanyl)-5-(methylthio)-1-(phenylsulfonyl)- | HCID 15486852 | 85% |
反応手順
To a solution of 2-benzenesulfonylamino-3-iodo-5-methylthiopyridine (1.60 g) in dioxane (40 ml), 2-ethynylfuran (725 mg), bis(triphenylphosphine) palladium chloride (138 mg), copper(I) iodide (75 mg) and triethylamine (598 mg) were added successively and the mixture was stirred in a sealed tube at 60° C. for 1 hour. 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 column chromatography (hexane:ethyl acetate=4:1) to obtain 1.24 g (85%) of the desired product as a brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07612070B2 |
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| 出典データセット | uspto-grants-2009_11 |
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| ORD ID | ord-a12745ff9f1c4a2f8d983518ef770b87 |
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| 出典メモ | uspto-grants-2009_11 |
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