関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4,4,5,5-Tetramethyl-2-(4-nitrophenyl)-1,3,2-dioxaborolane | HCID 2773555 | — |
| 反応物 | Methyl 2-(5-bromo-1,3-dioxoisoindolin-2-yl)-3-methylbutanoate | HCID 67305870 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 3-methyl-2-(5-(4-nitrophenyl)-1,3-dioxoisoindolin-2-yl)butanoate | HCID 67306305 | — |
反応手順
The compound of example 660 (2.5 g, 7.35 mmol); 4,4,5,5-tetramethyl-2-(4-nitrophenyl)-1,3,2-dioxaborolane (2.19 g, 8.82 mmol) and bis-Pinacolato diborane (180 mg, 0.22 mmol) were taken in dry DMF under argon atmosphere. Degassed 2M solution of sodium carbonate (1.94 g, 18.37 mmol) was added and the reaction mixture was heated to 80° C. for 2 h. The reaction mixture was cooled and the solvent was removed by distillation. The residue was taken in water and this aqueous mixture was extracted with ethyl acetate. The crude material was purified through column chromatography (silicagel, 30% dichloromethane in petroleum ether) to afford the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08748426B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-e03ec7b9187b408fa0405e470797cf3e |
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| 出典メモ | uspto-grants-2014_06 |
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