참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phenol | HCID 996 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-Methyl-2-nitrophenol | HCID 21026 | — |
| 반응물 | 2-Bromoethyl methyl ether | HCID 80972 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(2-Methoxy-ethoxy)-3-methyl-2-nitrobenzene | HCID 12855496 | — |
반응 단계
The required 1-(2-methoxy-ethoxy)-3-methyl-2-nitrobenzene was prepared from 3-methyl-2-nitrophenol. To a stirred solution of the phenol (2.0 g, 13.1 mmol) in DMF (65 mL) was added potassium carbonate (2.16 g, 15.7 mmol) and bromoethyl methyl ether (1.47 mL, 15.7 mmol) at room temperature. After the mixture was stirred at 50° C. for 48 h, water was added. The mixture was extracted with EtOAc (3×), washed with brine, dried over anhydrous MgSO4 filtered and evaporated. After chromatographic purification on silica gel, 1-(2-methoxy-ethoxy)-3-methyl-2-nitrobenzene was obtained in 85% yield (2.34 g). 1H NMR (500 MHz, CDCl3) δ 7.28 (1H, t, J=8.0 Hz), 6.89 (1H, d, J=9.0 Hz), 6.85 (1H, d, J=8.0 Hz), 4.19 (2H, t, J=4.5 Hz), 3.72 (2H, t, J=5.0 Hz), 3.41 (3H, s), 2.30 (3H, s).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08741942B2 |
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| 출처 데이터셋 | uspto-grants-2014_06 |
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| ORD ID | ord-5b8c2a2be6f74fb8b7a7f609036c07b5 |
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| 출처 메모 | uspto-grants-2014_06 |
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