反应详情

100.0 gm of fingolimod was dissolved in ethanol 250 ml and conc HCl 49 ml solutions. The reaction mass was stirred for about 30 min at room temperature; then concentrated under vacuum at about 40-45° C. 250 ml of ethanol was added. The reaction mass was heated to about 65-70° C. and 800 ml ethyl acetate was added in to reaction mass. The reaction mass was cooled to about 20-25° C. and stirred for about 30 min. The solid obtained was filtered and washed with ethyl, acetate to get 85 g of compound of Fingolimod hydrochloride. Purity 99.75% and Impurity compound of Formula XII: 0.06% by HPLC.

1. concentrationthen concentrated under vacuum at about 40-45° C
2. addition250 ml of ethanol was added
3. temperatureThe reaction mass was heated to about 65-70° C.
4. addition800 ml ethyl acetate was added in to reaction mass
5. temperatureThe reaction mass was cooled to about 20-25° C.
6. stirringstirred for about 30 min
7. customThe solid obtained
8. filtrationwas filtered
9. washwashed with ethyl, acetate