反应详情

17.0 gm of fingolimod was dissolved in (1:1) ethanol 120 ml:IPE.HCl 120 ml solutions. The reaction mass was stirred for about 30 min at room temperature; then concentrated under vacuum at about 40-45° C. 51 ml ethanol was added. The reaction mass was heated to about 50-55° C. and 200 ml ethyl acetate was added into the reaction mass. The reaction mass was cooled to about 5-10° C. and stirred for about 30 min. The solid obtained was filtered and washed with ethyl acetate to get 14.6 g of compound of Fingolimod hydrochloride. Purity 99.75% and regioisomer impurity compound of Formula IA: 0.006% by HPLC.

1. concentrationthen concentrated under vacuum at about 40-45° C
2. addition51 ml ethanol was added
3. temperatureThe reaction mass was heated to about 50-55° C.
4. addition200 ml ethyl acetate was added into the reaction mass
5. temperatureThe reaction mass was cooled to about 5-10° C.
6. stirringstirred for about 30 min
7. customThe solid obtained
8. filtrationwas filtered
9. washwashed with ethyl acetate