関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Triethyl phosphite | HCID 31215 | — |
| 反応物 | 1-(Chloromethyl)-2-(trifluoromethyl)benzene | HCID 89028 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Diethyl 2-(trifluoromethyl)benzylphosphonate | HCID 15818095 | — |
反応手順
To a suspension of sodium iodide (3.85 g, 25.6 mmol, 1 equiv.) in acetonitrile at room temperature under argon is added neat 1-chloromethyl-2-trifluoromethyl-benzene (commercially available from Acros Organics USA). To the resulting milky suspension is added freshly distilled triethyl phosphite (4.26 g, 25.6 mmol, 1 equiv.) and the resulting solution is stirred overnight at room temperature. After that time further triethyl phosphite (2.13 g, 12.9 mmol, 0.5 equiv.) is added and the reaction mixture heated at reflux for 1 hour. After cooling down to room temperature all volatiles were evaporated under reduced pressure. The residue is taken-up in dichloromethane and filtered through paper and the filtrate is concentrated under reduced pressure to yield the desired material as a clear oil pure enough to be used in the following step without further purification (7.46 g, 98%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07595315B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-866ca2e02fe7473f80b86807ac5b81a6 |
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| 出典メモ | uspto-grants-2009_09 |
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