反应详情

温度

65 °C

A mixture of (S)-2-[4-(3-fluorobenzyloxy)benzylamino]propanamide (20 g, 66 mmol, prepared in Example 12 a) and ethyl acetate (510 g) is heated, under stirring up to 65° C. and kept under these conditions until a clear solution is obtained. Methanesulfonic acid (7 g, 72.6 mmol) is added in 40 min to the solution precooled to 55° C. The mixture is gradually cooled to 20° C. in 3 hours, kept at 20° C. for 2 hours. The heterogeneous mixture is filtered, the solid is dried at reduced pressure at 40° C. to yield 26.1 g of title compound as white powder (99% yield).

1. temperatureis heated
2. customis obtained
3. customprecooled to 55° C
4. temperatureThe mixture is gradually cooled to 20° C. in 3 hours
5. filtrationThe heterogeneous mixture is filtered
6. customthe solid is dried at reduced pressure at 40° C.