反应详情

A mixture of acetic anhydride (27 ml) and formic acid (18.4 ml) was stirred at 50° for 135 minutes and then cooled to ambient temperature. 3'-Fluoro-2' (methylamino)acetophenone (20.48 g) was then added and the solution stirred overnight. Excess acetic formic anhydride was removed under reduced pressure at 30° and the residue then cooled to 5°. Water (92 ml) followed by aqueous sodium hydroxide (specific gravity 1.5) were then added dropwise to pH 7 whilst maintaining the temperature below 5°. The mixture was extracted with dichloromethane (3×35 ml) and the combined extracts were washed with saturated aqueous sodium carbonate (50 ml) then aqueous sodium chloride (6M, 50 ml) and dried over magnesium sulphate to give a solution of 2'-acetyl-6'-fluoro-N-methylformanilide.

1. stirringthe solution stirred overnight
2. customExcess acetic formic anhydride was removed under reduced pressure at 30°
3. temperaturethe residue then cooled to 5°
4. additionwere then added dropwise to pH 7
5. temperaturewhilst maintaining the temperature below 5°
6. extractionThe mixture was extracted with dichloromethane (3×35 ml)
7. washthe combined extracts were washed with saturated aqueous sodium carbonate (50 ml)
8. dry with materialaqueous sodium chloride (6M, 50 ml) and dried over magnesium sulphate