反应详情

温度

20 °C

5.03 g of 4-dimethylamino-pyridine were added to a solution of 16.5 g of the product of Step B in 205 ml of tetrahydrofuran and the mixture was stirred at 20° C. for 41/2 hours. The tetrahydrofuran was distilled off under reduced pressure at 40° C. and the dry residue wsa taken up in 500 ml of water. 42 ml of N hydrochloric acid were added to the mixture and the suspension was stirred at 20° C. for 30 minutes and was vacuum filtered. The product was washed with water, dried under reduced pressure at 70° C. and was crystallized from 310 ml of dioxane. The mixture was vacuum filtered at 15° C. and the product was washed with 30 ml of dioxane and dried under reduced pressure at 70° C. to obtain 13.3 g of 4-hydroxy-2-methoxymethyl-N-(2-thiazolyl)-8-trifluoromethyl-3-quinoline-carboxamide melting at 260° C.

1. distillationThe tetrahydrofuran was distilled off under reduced pressure at 40° C.
2. addition42 ml of N hydrochloric acid were added to the mixture
3. stirringthe suspension was stirred at 20° C. for 30 minutes
4. filtrationfiltered
5. washThe product was washed with water
6. customdried under reduced pressure at 70° C.
7. customwas crystallized from 310 ml of dioxane
8. filtrationfiltered at 15° C.
9. washthe product was washed with 30 ml of dioxane
10. customdried under reduced pressure at 70° C.