反应详情

温度

30 °C

A 4-neck RBF was charged under nitrogen flow with: 1 g of Midazolam (IV) (prepared according to example 2) and 15 mL of Ethanol. The slurry was stirred until complete dissolution at 25/30° C. 5 mL of a ethanolic solution of Hydrochloric acid 2N were slowly added. 20 mL of Isopropanol were added over 30 minutes at RT. The slurry was cooled down at −15° C. in one hour and kept at that temperature for at least 2 hours. The slurry was then filtered and the cake was washed with 10 mL of cool isopropanol. The filter was discharged and the product was dried at 40° C. under vacuum for 2 hours and then at 60° C. for 8 hours. Midazolam dihydrochloride as white solid was collected.

1. temperatureThe slurry was cooled down at −15° C. in one hour
2. waitkept at that temperature for at least 2 hours
3. filtrationThe slurry was then filtered
4. washthe cake was washed with 10 mL of cool isopropanol
5. customthe product was dried at 40° C. under vacuum for 2 hours
6. customMidazolam dihydrochloride as white solid was collected