反应详情

温度

100 °C

Dissolve 2-(4-chloro-phenyl)-5-[3-methoxy-4-(1-methyl-azetidin-3-yloxy)-phenyl]-5H-thiazolo[5,4-c]pyridin-4-one (638 mg, 1.41 mmol) in 1,4-dioxane at 100° C. To the above solution, add a solution of fumaric acid (5.64 mL, 1.41 mmol, 0.25 M in water). Stir the resulting solution at 100° C. for 5 min, then at 50° C. for one hour. Concentrate the solution with a stream of nitrogen gas to ¾ volume. Warm the mixture up to 100° C. until all the solids dissolve, then slowly cool to −10° C. Collect the white precipitate by filtration and wash the solids with cold dioxane (10 mL). Dry the solid at room temperature over the weekend to obtain 500 mg (62%) of the title compound as a fine white powder. ES/MS m/z (35Cl) 454 [M+1]+.

1. waitat 50° C. for one hour
2. concentrationConcentrate the solution with a stream of nitrogen gas
3. temperatureWarm the mixture up to 100° C. until all the solids
4. dissolutiondissolve
5. temperatureslowly cool to −10° C
6. customCollect the white precipitate
7. filtrationby filtration
8. washwash the solids with cold dioxane (10 mL)
9. customDry the solid at room temperature over the weekend