関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Chromanone | HCID 68110 | — |
| 反応物 | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(3,4-Dihydro-2H-4-chromenylidene)acetonitrile | HCID 56984834 | — |
反応手順
Diethyl cyanomethylphosphonate (1.15 eq.) is slowly added to a suspension of sodium hydride (1.15 eq.) in anhydrous tetrahydrofuran at 0° C. The reaction medium is stirred for 10 minutes at 0° C. and then cooled to −78° C. 4-Chromanone dissolved in tetrahydrofuran is added. The temperature is then returned slowly to 20-25° C. over 2 hours 30. After removal of the solvent, the compounds are extracted with ethyl acetate. The organic phase is washed with a large amount of a saturated solution of sodium chloride, concentrated and purified (Z/E mixture) on a silica column (AcOEt/PE 3/7).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06602903B2 |
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| 出典データセット | uspto-grants-2003_08 |
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| ORD ID | ord-c9307b8241da4fa28b5d39e90dbd41bb |
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| 出典メモ | uspto-grants-2003_08 |
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