反应详情

温度

90 °C

To a solution of ethyl 2-(2,6-dichloropyridin-3-ylamino)-2-oxoacetate (48.92 g, 186.0 mmol) in toluene (380 mL) was added Lawesson's Reagent (75.21 g, 186.0 mmol), and the resulting suspension was stirred at 90° C. for 4 h. The reaction mixture was then cooled to room temperature and filtered through Celite™, washing with 300 mL toluene. The combined filtrates were concentrated in vacuo at 40° C., and the residue was taken up in CH2Cl2 (200 mL) and filtered through a 200 g pad of silica gel, washing with additional CH2Cl2 (4×150 mL). The filtrate was concentrated in vacuo to afford ethyl 2-(2,6-dichloropyridin-3-ylamino)-2-thioxoacetate as an orange solid.

1. temperatureThe reaction mixture was then cooled to room temperature
2. filtrationfiltered through Celite™
3. washwashing with 300 mL toluene
4. concentrationThe combined filtrates were concentrated in vacuo at 40° C.
5. filtrationfiltered through a 200 g pad of silica gel
6. washwashing with additional CH2Cl2 (4×150 mL)
7. concentrationThe filtrate was concentrated in vacuo