関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Hydroxycoumarin | HCID 54682930 | — |
| 反応物 | 3,3,4,4,4-Pentafluorobutan-2-yl 4-formylbenzoate | HCID 58930722 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3,3,4,4,4-pentafluorobutan-2-yl 4-((4-hydroxy-2-oxo-2H-chromen-3-yl)methyl)benzoate | HCID 58760993 | 60% |
反応手順
Formic acid (35.8 ml) was added to 4-Hydroxycoumarin (15.8 g, 97.5 mmol) and aldehyde 3 (28.9 g, 97.6 mmol). Triethylamine (43 ml) was added (exothermic) at 0° C. It was warmed to 140° C. and stirred for 4 h at this temperature. The yellow solution was cooled to rt, ethyl acetate was added, it was washed with 1 N HCl and brine, it was dried over Na2SO4 and the solvent was removed. The slightly yellow solid was recrystallized from ethylacetate to yield the title compound as a white solid in 98% purity (60% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07253208B2 |
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| 出典データセット | uspto-grants-2007_08 |
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| ORD ID | ord-e4f7899bcd494527998cdc8695f7a6b3 |
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| 出典メモ | uspto-grants-2007_08 |
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