関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | 3-(Trimethylsilylethynyl)pyridine | HCID 4100857 | — |
| 反応物 | 1-Benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene | HCID 22504376 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-Benzenesulfonyl-5-methanesulfonyl-2-(3-pyridyl)indole | HCID 22504414 | 63% |
反応手順
A mixture of 3-trimethylsilylethynylpyridine (1.07 g), 2-benzenesulfonylamino-3-iodo-5-methanesulfonylbenzene (1.75 g), potassium acetate (1.60 g), cuprous iodide (60 mg), dichlorobis(triphenylphosphine)palladium (0.20 g) and 1,4-dioxane (4 ml) was stirred at 100° C. for 12 hours under nitrogen atmosphere. To the reaction solution were added water and ethyl acetate. The insolubles were filtered off. The filtrate was extracted with ethyl acetate, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography (hexane:ethyl acetate=1:3) to obtain 1.04 g of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06875770B2 |
|---|
| 出典データセット | uspto-grants-2005_04 |
|---|
| ORD ID | ord-fc99351053ee40dc8d49b302f8fd0440 |
|---|
| 出典メモ | uspto-grants-2005_04 |
|---|
