反应详情

温度

35 °C

A mixture of 24.0 g (147 mmol) of 4-chloro-2,6-difluoroaniline and 22.9 g of 1,2-propanediol was placed in a round bottom flask and heated to 35° C. with stirring. A mixture of 14.5 g (49 mmol) of 88 percent purity 2-chlorosulfonyl-8-fluoro-5-methoxy[1,2,4]triazolo[1,5-c]pyrimidine with 29.1 g of dichloromethane was prepared and was added in 1 mL shots over a 4 hour period. The resulting mixture was heated another 4 hours and was then stirred overnight at ambient temperature. It was then cooled to about 20° C. and filtered, collecting the solids present. The solids were slurried in 30 mL of a 1:1 mix of 2-propanol and water, collected by filtration, washed with 2×30 mL of 2-propanol, and air dried to obtain 14.8 g (75 percent of theory) of the title compound as a white powder of 98 percent purity melting at 203-204° C.

1. customwas placed in a round bottom flask
2. customwas prepared
3. additionwas added in 1 mL shots over a 4 hour period
4. temperatureThe resulting mixture was heated another 4 hours
5. stirringwas then stirred overnight at ambient temperature
6. temperatureIt was then cooled to about 20° C.
7. filtrationfiltered
8. customcollecting the solids present
9. additionmix of 2-propanol and water
10. filtrationcollected by filtration
11. washwashed with 2×30 mL of 2-propanol, and air
12. customdried