反应详情

温度

35 °C

A jacketed 250 mL (milliliter) round bottom flask equipped with a stirrer, condenser, and nitrogen inlet and outlet was loaded with 49.1 g (grams), 0.38 mol (mole) of 2,6-difluoroaniline and 25 g of 1,2-propanediol. The mixture was warmed to 35° C. by heating the jacket fluid and a solution of 30.3 g of 93 percent purity (0.10 mol) of 2-chlorosulfonyl-8-fluoro-5-methoxy[1,2,4]triazolo[1,5-c]pyrimidine in 30.2 g of dichloromethane was added portionwise with stirring under a nitrogen blanket over 3.5 hours. A solid began to form in about one hour and all of the chlorosulfonyl starting material was consumed in 5.5 hours. The resulting mixture was cooled to 20° C. and filtered, collecting the solids. The solids were washed 2×40 mL with methanol and then with 112 g of water. The white solid obtained after drying was found to be the title compound with a purity of greater than 99 percent and to amount to 34.2 g (88.9 percent of theory).

1. customA jacketed 250 mL (milliliter) round bottom flask equipped with a stirrer, condenser, and nitrogen inlet and outlet
2. temperatureby heating the jacket fluid
3. customto form in about one hour
4. customall of the chlorosulfonyl starting material was consumed in 5.5 hours
5. temperatureThe resulting mixture was cooled to 20° C.
6. filtrationfiltered
7. customcollecting the solids
8. washThe solids were washed 2×40 mL with methanol
9. customThe white solid obtained
10. customafter drying