反应详情

温度

90 °C

4-Chloro-3,5-bis(trifluoromethyl)benzamide (1.2 g, 1.0 eq.) was dissolved in toluene (20 mL) and Lawesson's reagent (3.32 g, 2.0 eq.) was added. The reaction mixture was stirred at 90° C. for 8 h then filtered. The filtrate was poured into water. The compound was extracted with EtOAc (3×100 mL). The combined organic layers was washed with brine (3×50 mL), dried over Na2SO4, filtered, and concentrated under reduced pressure (25° C., 20 mmHg) to afford 2 g of 4-chloro-3,5-bis(trifluoromethyl)benzothioamide (95% yield), which was used in the next step with no further purification.

1. filtrationthen filtered
2. additionThe filtrate was poured into water
3. extractionThe compound was extracted with EtOAc (3×100 mL)
4. washThe combined organic layers was washed with brine (3×50 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure (25° C., 20 mmHg)