関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrrole-2-carboxaldehyde | HCID 13854 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Bromomethyl-4-nitro-benzoic acid ethyl ester | HCID 13077445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-[2-Nitro-5-(ethoxycarbonyl)benzyl]-pyrrole-2-carboxaldehyde | HCID 21837115 | 83.9% |
反応手順
To a stirred slurry of 2.2 g of sodium hydride (60% in oil, washed with hexane) in tetrahydrofuran is added at 0° C. a solution of 4.5 g of pyrrole-2-carboxaldehyde in 25 ml of tetrahydrofuran. After the addition is complete, a solution of 15 g of ethyl 4-nitro-3-bromomethylbenzoate in 30 ml of dry tetrahydrofuran is slowly added under nitrogen. The reaction mixture is stirred at 20° C. for 8 hours and carefully quenched with water. The reaction mixture is extracted with chloroform which is washed with water, dried with Na2SO4 and concentrated in vacuo to give 12 g of the desired product as a solid; mass spectrum (M+ H)349.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05733905 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-169b2f504f264086a66d2edfe51fb873 |
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| 出典メモ | uspto-grants-1998_03 |
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