反应详情

A mixture of acetic anhydride (19.8 ml) and formic acid (13.5 ml) was stirred and heated at 60° under nitrogen for 2 hours. 1-(4-Fluoro-2-methylaminophenyl)-2-methylsulphonylethanone (10.0 g), was added portionwise to the mixture at ambient temperature with stirring. The mixture was stirred at 30° for 30 minutes. Water (30 ml) was added to the reaction mixture which was then stirred at 30° for 30 minutes. Concentration of the reaction mixture by evaporation in vacuo gave a green oil. The oil was dissolved in trichloromethane (50 ml) and washed with aqueous sodium hydrogen carbonate solution (7% w/w; 2×30 ml). The trichloromethane extract was dried (magnesium sulphate) and evaporated in vacuo to give a green oil which solidified at ambient temperature. Recrystallisation from toluene gave 5'-fluoro-N-methyl-2'-methylsulphonylacetylformanilide, m.p. 94.5°-95.5°.

1. temperatureheated at 60° under nitrogen for 2 hours
2. stirringwith stirring
3. stirringThe mixture was stirred at 30° for 30 minutes
4. stirringwas then stirred at 30° for 30 minutes
5. customConcentration of the reaction mixture by evaporation in vacuo
6. customgave a green oil
7. washwashed with aqueous sodium hydrogen carbonate solution (7% w/w; 2×30 ml)
8. extractionThe trichloromethane extract
9. dry with materialwas dried (magnesium sulphate)
10. customevaporated in vacuo
11. customto give a green oil which
12. customsolidified at ambient temperature
13. customRecrystallisation from toluene