反应详情

温度

60 °C

The product of Example I was dissolved in anhydrous ethanol. The solution was heated to 60° C. Methanesulfonic acid was added at this temperature and a white slurry formed. The slurry was cooled to 0 to 5° C. over 1 hour and stirred for an additional 1 hour. The resulting white crystalline solid was filtered and washed with cold anhydrous ethanol. The wet cake was dried in a vacuum oven at 70° C. until the loss on drying (LOD) was <0.5% to afford the title product as a white, crystalline substance (13.2 g, 92.3% yield, HPLC AP >99). Typical yield is between about 92% to about 97%.

1. customa white slurry formed
2. temperatureThe slurry was cooled to 0 to 5° C. over 1 hour
3. filtrationThe resulting white crystalline solid was filtered
4. washwashed with cold anhydrous ethanol
5. customThe wet cake was dried in a vacuum oven at 70° C. until the loss
6. customon drying (LOD)