反应详情

A mixture of methyl 2-[N-(4-fluorophenyl)carbamoyl]acetate (10 g), carbon disulfide (3.2 ml) and acetone (200 ml) was cooled to 5°-10° C., to which 50% aqueous sodium hydroxide (4.2 ml) was added dropwise. The mixture was stirred at same temperature for 2 hrs, then dibromomethane (4 ml) was added dropwise and the reaction mixture was stirred at room temperature for 1 hr and refluxed for 2 hrs. The solid was removed by filtration and the filtrate was poured onto ice-water. The solid formed was filtered, and dissolved in methylene chloride. The solution was washed with 10% aqueous sodium hydroxide solution and water, then dried. The solvent was evaporated and the residue was purified with ethyl acetate and ethyl ether to give the titled compound as a white solid. (8.5 g, 60%).

1. additionwas added dropwise
2. stirringthe reaction mixture was stirred at room temperature for 1 hr
3. temperaturerefluxed for 2 hrs
4. customThe solid was removed by filtration
5. additionthe filtrate was poured onto ice-water
6. customThe solid formed
7. filtrationwas filtered
8. dissolutiondissolved in methylene chloride
9. washThe solution was washed with 10% aqueous sodium hydroxide solution and water
10. customdried
11. customThe solvent was evaporated
12. customthe residue was purified with ethyl acetate and ethyl ether