反应详情

温度

90 °C

To a solution of 4-chloro-3,5-bis(trifluoromethyl)benzamide (1.2 g) in toluene (20 mL) was added Lawesson's reagent (3.32 g, 2.0 eq.). The reaction mixture was stirred at 90° C. for 8 h before being cooled to room temperature and filtered. The filtrate was poured into water and extracted with EtOAc (3×100 mL). The combined organic extracts were washed with brine (3×50 mL), dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure (25° C., 20 mmHg) to afford 2 g of crude compound. The crude compound was purified by combi-flash chromatography (eluting with 7% EtOAc:hexane) to afford 1.0 g of desired compound (yield: 79%).

1. temperaturebefore being cooled to room temperature
2. filtrationfiltered
3. additionThe filtrate was poured into water
4. extractionextracted with EtOAc (3×100 mL)
5. washThe combined organic extracts were washed with brine (3×50 mL)
6. dry with materialdried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure (25° C., 20 mmHg)
9. customto afford 2 g of crude compound
10. customThe crude compound was purified by combi-flash chromatography (eluting with 7% EtOAc:hexane)