反应详情

温度

100 °C

N-(1-Hydroxy-2-(hydroxymethyl)-4-(4-octylphenyl)butan-2-yl) acetamide (23.5 g) is charged into a 250 mL single-neck round bottom flask equipped with a condenser and 3N hydrochloric acid (100 mL) is added. The mixture is heated to 100° C. and stirred for 3 hours. The mass is cooled to room temperature and maintained overnight. The mass is extracted with ethyl acetate (3×100 mL) and the ethyl acetate extracts are combined, dried with sodium sulphate, and concentrated under vacuum to produce a gummy solid. Ethanolic hydrochloride solution is added to the solid, stirred for 3 hours at room temperature and the obtained solid is separated by filtration and suction dried. The solid is recrystallized from an isopropyl alcohol solution to give fingolimod hydrochloride. Yield: 5.7 g.

1. customequipped with a condenser
2. temperatureThe mass is cooled to room temperature
3. temperaturemaintained overnight
4. extractionThe mass is extracted with ethyl acetate (3×100 mL)
5. dry with materialdried with sodium sulphate
6. concentrationconcentrated under vacuum
7. customto produce a gummy solid
8. stirringstirred for 3 hours at room temperature
9. customthe obtained solid is separated by filtration and suction
10. customdried
11. customThe solid is recrystallized from an isopropyl alcohol solution