関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Diphenyl (phenylamino)(pyridin-4-yl)methylphosphonate | HCID 423769 | — |
| 反応物 | 614729-75-8 | HCID 22247846 | — |
| 溶媒 | 2-Furanpropanol, tetrahydro- | HCID 13020 | — |
| 生成物 | HCID 22248020 | HCID 22248020 | 36% |
反応手順
After dissolving 19.6 g of [(phenylamino)-(4-pyridylmethyl)]phosphonic acid diphenyl ester [CAS No.3360-72-3] in 115 ml of tetrahydrofuran-2-propanol (4:1), 6.02 g of 4-fluorothiophene-3-carboxaldehyde and 19.61 g of anhydrous cesium carbonate were added and the mixture was stirred overnight at room temperature. Next, 90 ml of 5N hydrochloric acid was added to the reaction mixture and the mixture was stirred at room temperature for 6 hours. After adding a 5N sodium hydroxide solution to the reaction solution, extraction was performed with ethyl acetate. The organic layer was washed with water and saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate). The obtained solid was washed with n-hexane to obtain the title compound (3.66 g, 36% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06995144B2 |
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| 出典データセット | uspto-grants-2006_02 |
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| ORD ID | ord-62ad8f8894364847877351c556aca5cb |
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| 出典メモ | uspto-grants-2006_02 |
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