関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propanal | HCID 527 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Methyl 4-(diethylphosphorylmethyl)benzoate | HCID 21989718 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | methyl (E)-4-(but-1-en-1-yl)benzoate | HCID 12737446 | — |
反応手順
To a suspension of sodium hydride (60%, 0.97 g) in tetrahydrofuran (80 mL) was added methyl 4-(diethylphosphorylmethyl)benzoate (5.8 g) at 0° C., and the mixture was stirred for 30 minutes. To the reaction mixture was added a solution of propionaldehyde (1.6 mL) in tetrahydrofuran (10 mL), and the mixture was stirred at room temperature for 30 minutes. To the reaction mixture was added a saturated aqueous ammonium chloride solution, and the mixture was extracted with diethyl ether. The organic layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=5/1) to give methyl (E)-4-(but-1-en-1-yl)benzoate (2.5 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087579B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-6e4a81ed99724d89ab0593aba47b36bc |
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| 出典メモ | uspto-grants-2006_08 |
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