関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | (5-Acetylthiophen-2-yl)boronic acid | HCID 4143377 | — |
| 反応物 | 3-(5-Bromopyridine-3-carbonyl)-1-methylpyrrolidin-2-one | HCID 14061371 | — |
| 触媒 | Ferrocene-1,1'-bis-(diphenylphosphine) | HCID 635956 | — |
| 溶媒 | Dioxane toluene | HCID 21840791 | — |
| 生成物 | 3-(5-(5-Acetylthiophen-2-yl)nicotinoyl)-1-methylpyrrolidin-2-one | HCID 71570118 | 50% |
反応手順
A mixture of 3-(5-bromonicotinoyl)-1-methylpyrrolidin-2-one 3 (1 equiv), 5-Acetyl-2-thiopheneboronic acid (1.2 equiv), 1,1′-bis(diphenylphosphino)ferrocene]dichloro palladium(II) complex with DCM (0.1 equiv) and 2M Na2CO3(4 equiv) in toluene/1,4-dioxane(4:1, 15 volumes) was degassed and filled with nitrogen. Then the reaction mixture was heated to 85° C. and maintained for 2 h. After completion of the reaction filtered through Celite bed and washed with ethyl acetate. The combined organic layer was dried over with anhydrous sodium sulfate, filtered and concentrated under reduced pressure to obtain crude residue which was purified by silica-gel column chromatography using 2% MeOH/DCM as an eluent to afford 50% yield of titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835640B1 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-bee8575046a648daae173e0b9e6482e5 |
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| 出典メモ | uspto-grants-2014_09 |
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