関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Nitrophenol | HCID 980 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-(2-(2-Methoxyethoxy)ethoxy)ethyl 4-methylbenzenesulfonate | HCID 9948898 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-{2-[2-(2-Methoxyethoxy)ethoxy]ethoxy}-4-nitrobenzene | HCID 14691822 | 94.7% |
反応手順
To a stirred solution of 16 (1.83 g, 5.75 mmol) in anhydrous DMF (10 mL) were added K2CO3 (2.39 g, 17.3 mmol) and 4-nitrophenol (0.78 g, 5.59 mmol), and the reaction mixture was heated to 80° C. for 16 h. After cooling, the mixture was diluted in water, extracted three times with DCM, and then dried over MgSO4. The filtrate was concentrated under reduced pressure to give an oily residue, which was purified by flash chromatography over silica gel with Hex/EtOAc (1:2) to afford 17 as a yellow oil (1.51 g, 92%): 1H NMR (500 MHz, CDCl3) δ 8.19 (d, J=9.1 Hz, 2H), 6.97 (d, J=9.1 Hz, 2H), 4.26-3.65 (m, 12H), 3.37 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841460B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-2394a121b57540eea619009698c28bfe |
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| 出典メモ | uspto-grants-2014_09 |
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