反应详情

A mixture of acetic anhydride (26.5 ml) and formic acid (98%, 17.4 ml) was stirred at 50°-60° for 110 minutes and then cooled to ambient temperature. 4'-Fluoro-2'-(methylamino)acetophenone (19.9 g) was added and the mixture stirred overnight at ambient temperature. Water (90 ml) was added and the mixture stirred in an ice/ salt bath. Aqueous sodium hydroxide (specific gravity 1.5, 50 ml) was added dropwise over a period of 30 minutes whilst maintaining the temperature below 30°. The mixture was extracted with dichloromethane (3×50 ml) and the combined extracts were dried over magnesium sulphate to give a solution of 2'-acetyl-5'-fluoro-N-methylformanilide.

1. stirringthe mixture stirred overnight at ambient temperature
2. stirringthe mixture stirred in an ice/ salt bath
3. temperaturewhilst maintaining the temperature below 30°
4. extractionThe mixture was extracted with dichloromethane (3×50 ml)
5. dry with materialthe combined extracts were dried over magnesium sulphate