反应详情

温度

70 °C

A mixture of 1-bromo-1-(4-fluoro-3-methanesulfonyl-phenyl)-propan-2-one (Example 47c) (0.17 g, 0.55 mmol) and N-acetylthiourea (0.065 g, 0.55 mmol) in ethanol is heated at 70° C. for 3 hours then at room temperature over two days. The reaction mixture is poured into water (200 ml) and extracted with ethyl acetate (3×50 ml). The combined organic layers are dried over MgSO4, filtered and concentrated to afford a viscous solid. This solid in a minimum amount of ethyl acetate is sonicated to give a suspension which is then heated until all solid has dissolved then left to cool to room temperature overnight. The white crystalline solid is filtered off to afford the titled compound.

1. extractionextracted with ethyl acetate (3×50 ml)
2. dry with materialThe combined organic layers are dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customto afford a viscous solid
6. customto give a suspension which
7. temperatureis then heated until all solid
8. dissolutionhas dissolved
9. waitthen left
10. temperatureto cool to room temperature overnight
11. filtrationThe white crystalline solid is filtered off