N-bromobutanimide → HCID 71237985、化合物
反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([F:9])=[C:5]([O:10][CH3:11])[CH:4]=1)[CH3:2].C1C(=O)N([Br:19])C(=O)C1>CC#N>[Br:19][C:8]1[CH:7]=[C:6]([F:9])[C:5]([O:10][CH3:11])=[CH:4][C:3]=1[CH2:1][CH3:2]参加物
4
実験手順
To a solution of 4-ethyl-1-fluoro-2-methoxy-benzene (WO-2010/090537, 12.2 g, 79.1 mmol) in MeCN (150 mL) was added a solution of NBS (14.4 g, 80.7 mmol) in MeCN (50 mL). The resulting solution was stirred at room temperature for 18 hours. The solvent was removed in vacuo and the residue was diluted with diethyl ether (150 mL). Precipitated solid was removed by filtration and the filtrate was washed with sodium sulfite aqueous solution (100 mL) and brine (100 mL), dried over MgSO4 and concentrated in vacuo to give the title compound as a yellow oil (18 g) in a 97% yield.
後処理
- customThe solvent was removed in vacuo
- additionthe residue was diluted with diethyl ether (150 mL)
- customPrecipitated solid
- customwas removed by filtration
- washthe filtrate was washed with sodium sulfite aqueous solution (100 mL) and brine (100 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-840014a801d749a1a494ab377d854ff1
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08575336B2
反応ノート
読み込み中…