Iodide Ion → Methyl 2'-fluoro-5'-iodo-4'-methoxy-3-methylbiphenyl-4-carboxylate
反応式
[F:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][C:13]([C:16]([O:18][CH3:19])=[O:17])=[C:12]([CH3:20])[CH:11]=1.[I-:21]>S([O-])([O-])(=O)=O.[Ag+2].CO>[F:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([I:21])=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][C:13]([C:16]([O:18][CH3:19])=[O:17])=[C:12]([CH3:20])[CH:11]=1参加物
5
実験手順
methyl 2′-fluoro-4′-methoxy-3-methylbiphenyl-4-carboxylate (100 mg, 0.365 mmol), methanol (3 mL), iodide (93 mg, 0.366 mmol) and silver sulfate (114 mg, 0.366 mmol) were stirred at room temperature for 1.5 hours. Reaction crude was quenched by Na2SO3 (sat., aq.). Volatiles were removed from the grayish brown mixture. The pot residue was worked up with H2O/EtOAc/Na2SO4/filtration/concentration to afford the title compound. LCMS (ESI) calc.=400.00; found=400.96 (M+1)+.
後処理
- customReaction crude
- customwas quenched by Na2SO3 (sat., aq.)
- customVolatiles were removed from the grayish brown mixture
- concentrationThe pot residue was worked up with H2O/EtOAc/Na2SO4/filtration/concentration
出典と根拠
- ORDレコード
- ord-a7351fc43371436a854e1fd6028cd7e8
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08440702B2
反応ノート
読み込み中…