反应详情

温度

20 °C

A solution of Saxagliptin (monohydrate, 4.5 g) in 1-butanol (“1-BuOH”, 68 ml) was warmed up to 40° C. and conc. Conc. HCl was added (1.258 ml). The resulting mixture was stirred at the same temperature for 30 min and a suspension was formed. The suspension was cooled to 20° C. and butyl acetate (“BuOAc” 68 ml) was added dropwise. The suspension was cooled to 0° C. and stirred for 2 h. The suspension was filtered, and the collected crystalline solid was washed with cool 1-BuOH/BuOAc (1/1) mixture yielding 3.92 g of the product. PXRD is shown in FIG. 18.

1. customa suspension was formed
2. temperatureThe suspension was cooled to 0° C.
3. stirringstirred for 2 h
4. filtrationThe suspension was filtered
5. washthe collected crystalline solid was washed with cool 1-BuOH/BuOAc (1/1) mixture