関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methyloxybenzyl chloride | HCID 69993 | — |
| 反応物 | Cyclopropanecarbonitrile | HCID 79637 | — |
| 反応物 | 1-(4-methoxy-benzyl)-cyclopropanecarbonitrile Sodium bis(trimethylsilyl)amide | HCID 86603547 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(4-Methoxy-benzyl)-cyclopropanecarbonitrile | HCID 57456950 | — |
反応手順
1-(4-Methoxy-benzyl)-cyclopropanecarbonitrile Sodium bis(trimethylsilyl)amide (2 M in tetrahydrofuran, 37.5 mL, 75.0 mmol) was slowly added to a solution of cyclopropanecarbonitrile (3.35 g, 49.9 mmol) in THF (30 mL) at room temperature. The reaction mixture was stirred for 20 minutes and then a solution 1-chloromethyl-4-methoxy-benzene (7.83 g, 50.0 mmol) in THF was added. The mixture was heated at reflux for 3 hours and then quenched with a saturated aqueous solution of ammonium chloride (50 mL). The separated aqueous layer was extracted three times with ethyl acetate (50 mL). The combined organic layers were washed with a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride, dried over sodium sulfate, filtered, and evaporated to dryness to give crude 1-(4-methoxy-benzyl)-cyclopropanecarbonitrile, which was used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541453B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-fbc156986c084e01b76995a2830ab6c6 |
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| 出典メモ | uspto-grants-2013_09 |
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