反应详情

A mixture of acetic anhydride (4.6 ml) and formic acid (3.1 3 ml) was stirred at 60° for 2 hours and then cooled to 10°. 5'-Fluoro-2'-(methylamino)acetophenone (3.0 g) was then added and the mixture stirred overnight. The solution was cooled in an ice-bath and water (20 ml) added followed by aqueous sodium hydroxide (specific gravity 1.5) added dropwise to pH 10. The mixture was extracted with dichloromethane (3×30 ml) and the combined extracts dried over magnesium sulphate to give a solution of 2'-acetyl-4'-fluoro-N-methylformanilide.

1. temperaturecooled to 10°
2. stirringthe mixture stirred overnight
3. temperatureThe solution was cooled in an ice-bath
4. additionadded dropwise to pH 10
5. extractionThe mixture was extracted with dichloromethane (3×30 ml)
6. dry with materialthe combined extracts dried over magnesium sulphate