関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methanone, [1-(2-chloroethyl)-4-piperidinyl](4-fluorophenyl)- | HCID 10516150 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 2-acetyl-4-[4-(4-fluorobenzoyl)piperidino]-butyrate | HCID 14882705 | — |
反応手順
A solution of 5.45 g of ethyl acetoacetate in 20 ml of tetrahydrofuran is added at 0° C. to a suspension of 1.68 g of sodium hydride at a concentration of 60% in oil in 100 ml of anhydrous tetrahydrofuran. The medium is maintained at 20° C. for 1 hour 30 minutes. 6.3 g of sodium iodide are added, followed by the addition at 0° C. of 11.3 g of 1-(2-chloroethyl)-4-(4-fluorobenzoyl)piperidine in 100 ml of tetrahydrofuran. The reaction mixture is brought to reflux for 15 hours. It is concentrated under vacuum. The residue is taken up in water and the product is extracted with dichloromethane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05077288 |
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| 出典データセット | uspto-grants-1991_12 |
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| ORD ID | ord-eb99b06868674e2c9d29b38620f253b3 |
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| 出典メモ | uspto-grants-1991_12 |
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