Dimethylformamide → 4-Formyl-2-methoxybenzonitrile
反応式
FC(F)(F)S(O[C:7]1[CH:12]=[CH:11][C:10]([CH:13]=[O:14])=[CH:9][C:8]=1[O:15][CH3:16])(=O)=O.CCOC(C)=O.[CH3:25][N:26](C=O)C>[C-]#N.[Zn+2].[C-]#N>[CH:13]([C:10]1[CH:11]=[CH:12][C:7]([C:25]#[N:26])=[C:8]([O:15][CH3:16])[CH:9]=1)=[O:14]参加物
5
反応条件
- 温度
- 110 °C
実験手順
A mixture of 4-formyl-2-methoxyphenyl trifluoromethanesulfonate (37.0 g, 130 mmol), zinc cyanide (61.0 g, 521 mmol) and tetrakis triphenylphosphine palladium (0) (22.6 g, 19.5 mmol) in DMF (300 mL) were stirred at 110° C. for 8 h. EtOAc was added to the reaction mixture and the organic layer was washed two times with water, dried, filtered and concentrated. The crude product was then purified by column chromatography (silica gel, ethylacetate/hexanes 3:7) which afforded 4-formyl-2-methoxybenzonitrile.
後処理
- washthe organic layer was washed two times with water
- customdried
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was then purified by column chromatography (silica gel, ethylacetate/hexanes 3:7) which
出典と根拠
- ORDレコード
- ord-027cf47f1fc44dc88b16f73748747088
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08673920B2
反応ノート
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