Sulfuric Acid → 2-Ethyl-6-nitroaniline
반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[C:4]=1[NH:12]C(=O)C)[CH3:2].OS(O)(=O)=O>O>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[C:4]=1[NH2:12])[CH3:2]참가 물질
4
실험 절차
A mixture of crude N-(2-ethyl-6-nitrophenyl)acetamide (2.4 g, 12 mmol), H2SO4 (3.4 g, 36 mmol), and H2O (10 mL) was refluxed for 2 hours and steam distilled. The distillate was extracted with Et2O and the organic phase was washed with brine and dried over Na2SO4. The solvent was evaporated to give the title compound as a yellow liquid (0.5 g, 25%). 1H NMR (400 MHz, CD3OD) δ 7.95 (1H, d, J=8.8 Hz), 7.31 (1H, d, J=6.8 Hz), 6.62 (1H, dd, J=8.8, 7.6 Hz), 2.63 (2H, q, J=7.6 Hz), 1.27 (3H, t, J=7.6 Hz).
후처리
- temperaturewas refluxed for 2 hours
- distillationsteam distilled
- extractionThe distillate was extracted with Et2O
- washthe organic phase was washed with brine
- dry with materialdried over Na2SO4
- customThe solvent was evaporated
출처 및 근거
- ORD 기록
- ord-2c2ed0de9b694dcba6d466a15b734451
- 출처 데이터셋
- uspto-grants-2016_06
- 특허 번호
- US09365566B2
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