Iodoethane → 4-Bromo-1-ethoxy-2-nitrobenzene
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:18](I)[CH3:19]>CC(=O)CC>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:18][CH3:19])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1参加物
5
実験手順
4-Bromo-2-nitrophenol (5.0 g, 23 mmol) and potassium carbonate (9.52 g, 69 mmol) were suspended in 2-butanone (100 ml). Ethyl iodide (2.2 ml, 28 mmol) was added dropwise at room temperature and stirred for 30 minutes. The suspension was heated at reflux for 18 hours, cooled and filtered, and the residue washed with acetone. The filtrate was concentrated in vacuo to a crude solid that was used without further purification (D14). 1H-NMR (CDCl3) δ 7.42 (1H, d, J 2.5 Hz), 7.60 (1H, dd, J 9.0, 2.5 Hz), 6.96 (1H, d, J 9.0 Hz), 4.17 (2H, q, J 7.0 Hz), 1.47 (3H, t, J 7.0 Hz).
後処理
- temperatureThe suspension was heated
- temperatureat reflux for 18 hours
- temperaturecooled
- filtrationfiltered
- washthe residue washed with acetone
- concentrationThe filtrate was concentrated in vacuo to a crude solid that
- customwas used without further purification (D14)
出典と根拠
- ORDレコード
- ord-fb9bc193cfa74a289e987198dbf5bdf9
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07381728B2
反応ノート
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