関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,3-Dichloro-5-(trifluoromethyl)pyridine | HCID 112234 | — |
| 反応物 | Methyl [o-(5-hydroxy-2-nitrophenoxy)phenoxy]acetate | HCID 54060386 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl {o-{5-{[3-chloro-5-(trifluoromethyl)-2-pyridyl]oxy}-2-nitrophenoxy}phenoxy}acetate | HCID 54238225 | 27.2% |
反応手順
A mixture of methyl [o-(5-hydroxy-2-nitrophenoxy)phenoxy]acetate (1.9 g, 5.9 mmol), 2,3-di-chloro-5-(trifluoromethyl)pyridine (1.92 g, 8.9 mmol) and potassium carbonate (1.23 g, 8.9 mmol) in N,N-di-methylformamide is heated at 100° C. for 12 hours, cooled to room temperature, poured into water and extracted with ether. The organic extract is washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain a yellow oil. Flash chromatography of the oil using silica gel and a (1:4) ethyl acetate/hexanes solution gives the title product as a yellow liquid (0.8 g) which is identified by 1HNMR and 13CNMR spectral analyses.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424280 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-0ea58b021f504387a450c1fee6fddaa9 |
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| 出典メモ | uspto-grants-1995_06 |
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