反应详情

To a solution of 5-fluoro-4-(2-hydroxyethyl)-2-methoxybenzonitrile (175 mg, 0.90 mmol) in dichloromethane (4 mL) was added Dess-Martin periodinane (530 mg, 1.3 mmol) at RT. The mixture stirred at roomtemperature for 2 h, then was diluted with saturated sodium bicarbonate and saturated sodium thiosulfate and stirred 30 min. The mixture was extracted with dichloromethane (3×) and the combined organics dried (MgSO4), filtered and concentrated to provide 5-fluoro-2-methoxy-4-(2-oxoethyl)benzonitrile which was used without further purification. LC-MS (IE, m/z): 194.2 [M+1]+.

1. stirringstirred 30 min
2. extractionThe mixture was extracted with dichloromethane (3×)
3. dry with materialthe combined organics dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated