反应详情

温度

10 °C

1-(3-Fluoro-4-methanesulfonyl-phenyl)-propan-2-one (68c) (6.0 g, 26 mmol) is dissolved in dioxan (50 ml) and the solution is cooled to 10° C. at which point the mixture is semi frozen. A solution of bromine (0.9 ml, 17 mmol) in chloroform (2 ml) is added slowly over 30 minutes and the mixture is stirred for an additional 15 minutes in a semi frozen state. The mixture is then allowed to warm to room temperature and the solvent is removed to give a red oil. Ethanol (70 ml) and (1H-pyrazol-3-yl)-thiourea (35a) (3.2 g, 22 mmol) are added and the reaction is stirred at 60° C. for 30 minutes. The solution is allowed to cool to room temperature whereupon the product crystallises. Filtration affords the titled compound.

1. temperatureis semi frozen
2. temperaturefrozen state
3. temperatureto warm to room temperature
4. customthe solvent is removed
5. customto give a red oil
6. stirringthe reaction is stirred at 60° C. for 30 minutes
7. temperatureto cool to room temperature whereupon the product
8. customcrystallises
9. filtrationFiltration