참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Allyl iodide | HCID 11166 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 7-Fluoro-1,5-naphthyridin-2(1H)-one | HCID 46900801 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 7-Fluoro-1-(2-propen-1-yl)-1,5-naphthyridin-2(1H)-one | HCID 58579467 | 63% |
반응 단계
7-Fluoro-1,5-naphthyridin-2(1H)-one (2.152 g, 13.122 mmol) was suspended in dry DMF (40 ml) under argon at 0° C., and the stirred suspension was treated with sodium hydride (1.155 g of a 60% w:w dispersion in oil, 2.2 eq.) added in portions. The suspension was allowed to warm to rt. After stirring for 30 mins at rt, the mixture was treated with allyl iodide (2.67 ml, 2.2 eq) and then stirred for a further 30 min before addition of water (100 ml). The mixture was then extracted with DCM (3×200 ml). The organic extracts were combined, dried over anhydrous magnesium sulphate, filtered and evaporated to give a residue which was purified by column chromatography on silica with a 0-10% methanol in DCM gradient to give the desired product as a light brown solid (1.683 g, 63%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08071592B2 |
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| 출처 데이터셋 | uspto-grants-2011_12 |
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| ORD ID | ord-99fd1e59768d4e9d81031f9de5e50b74 |
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| 출처 메모 | uspto-grants-2011_12 |
|---|