反应详情

14.1 g of anhydrous methanesulfonic acid were added to a stirred mixture of 63.2 g of doxazosin, 125 ml of N-methyl-2-pyrrolidone and 500 ml of methanol in a 1 l three-neck round-bottom flask. The internal temperature rose to 30° C. during this, and a solution was produced. After the addition of methanesulfonic acid was complete, the reaction mixture was filtered into a second 1 l three-neck round-bottom flask. The filter was washed with 85 ml of methanol, and the combined filtrates were stirred for 5 h. After the end of the stirring time, the resulting precipitate was filtered off with suction and washed 3× with 25 ml of methanol each time. 125 g of moist doxazosin mesylate (modification D) were obtained. This corresponds to 70.4 g of dry substance and a yield of 91.8%.

1. customrose to 30° C.
2. customwas produced
3. filtrationthe reaction mixture was filtered into a second 1 l three-neck round-bottom flask
4. washThe filter was washed with 85 ml of methanol
5. filtrationAfter the end of the stirring time, the resulting precipitate was filtered off with suction
6. washwashed 3× with 25 ml of methanol each time