関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Lactate | HCID 7344 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4-Difluoronitrobenzene | HCID 67967 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Ethyl 2-(5-fluoro-2-nitrophenoxy)propanoate | HCID 19786322 | — |
反応手順
2,4-Difluoronitrobenzene (15.9 g; 0.10 mole), ethyl lactate (11.8 g; 0.10 mole), and anhydrous potassium carbonate (13.8 g, 0.10 mole) are combined in dioxane (200 ml) and the temperature is brought to 95° C. over a 1.5 hour period and maintained at 95° C. for 3 hours. The reaction mixture is cooled to room temperature, the inorganic solids removed by filtration and the solvent removed under vacuum to afford a dark colored oil, from which low boiling fractions are removed by distillation (bp., 79° C./0.5 mm). The pot residue is then cooled to afford 15.9 g of crude product, which is recrystallized from ligroin/acetone to afford ethyl 2-(5-fluoro-2-nitrophenoxy)propionate as yellow needles, m.p. 64°-65° C. Elemental anal. Calcd for C11H12FNO5 : C, 51.4; H, 4.70; F, 7.38; N, 5.45. Found: C, 51.35; H, 4.74; F, 7.60; N, 5.44.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04262152 |
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| 出典データセット | uspto-grants-1981_04 |
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| ORD ID | ord-4db2e06b44154f19b9406b2626e69f5d |
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| 出典メモ | uspto-grants-1981_04 |
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