Methanol → HCID 20577071、化合物
反応式
[Br:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([F:14])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].O=S(Cl)Cl.[CH3:19]O>>[Br:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([F:14])=[CH:7][C:3]=1[C:4]([O:6][CH3:19])=[O:5]参加物
4
反応条件
- 温度
- 65 °C
実験手順
To the solution of 2-bromo-5-fluoro-3-nitrobenzoic acid (35 g) in MeOH (400 mL) was added SOCl2 (40 mL) drop-wise at 10-15° C. The reaction was then stirred at 65° C. for 1 h. After cooling to room temperature, the solvent was evaporated in vacuum to afford a residue, which was chromatographed on silica gel using gradient eluant of 0-100% EtOAc in hexane to provide methyl 2-bromo-5-fluoro-3-nitrobenzoate (20 g, 84%).
後処理
- temperatureAfter cooling to room temperature
- customthe solvent was evaporated in vacuum
- customto afford a residue, which
- customwas chromatographed on silica gel using gradient eluant of 0-100% EtOAc in hexane
出典と根拠
- ORDレコード
- ord-67a2b8a66da548e8acde762fba7b729a
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09328111B2
反応ノート
読み込み中…