反应详情

温度

20 °C

19.2 g crude terbinafine base (57.2 mmol theoretical, example 6) is dissolved in 83 ml acetone and then 6.2 ml (0.0631 mol) of 32% aqueous hydrochloric acid is added dropwise. The resulting suspension is stirred for 30 minutes at 20° C. and then cooled to −5°/−10° C. and stirred for a further 2.5 hours. The precipitate is filtered, washed with 16 ml cold acetone and dried to constant weight at 40° C. in a vacuum oven. 10.8 g (57.5% yield) terbinafine-HCl is obtained as a white solid with purity in excess of 99.8% (HPLC A %).

1. temperaturecooled to −5°/−10° C.
2. stirringstirred for a further 2.5 hours
3. filtrationThe precipitate is filtered
4. washwashed with 16 ml cold acetone
5. customdried to constant weight at 40° C. in a vacuum oven