참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Acetate | HCID 517044 | — |
| 반응물 | 2-Benzenesulfonylamino-3-iodo-5-methylthiopyridine | HCID 15486851 | — |
| 반응물 | 5-Ethoxycarbonyl-2-trimethylsilylethynylpyridine | HCID 22504397 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 6-(1-Benzenesulfonyl-5-methylthio-1h-pyrrolo[2,3-b]pyridin-2-yl)nicotinic acid ethyl ester | HCID 68444739 | 98.5% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06875770B2 |
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| 출처 데이터셋 | uspto-grants-2005_04 |
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| ORD ID | ord-0f1fd7e7c0f54fbc91234c3ff00dc5b1 |
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| 출처 메모 | uspto-grants-2005_04 |
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