Sulfuric Acid → 2-Ethyl-6-nitroaniline
反応式
[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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-2c2ed0de9b694dcba6d466a15b734451
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09365566B2
反応ノート
読み込み中…