참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Chromanone | HCID 68110 | — |
| 반응물 | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(3,4-Dihydro-2H-4-chromenylidene)acetonitrile | HCID 56984834 | — |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06313160B1 |
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| 출처 데이터셋 | uspto-grants-2001_11 |
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| ORD ID | ord-a8d847581f8746b59b832d47f4769ed2 |
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| 출처 메모 | uspto-grants-2001_11 |
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