反应详情

To 14.1 g (0.04 mol) of 3-(hydroxymethyl)-3-nitro-1-(p-octylphenyl)butane-1,4-diol in 250 ml of methyl alcohol, 30 ml of concentrated hydrochloric acid was added, followed by the catalyst—10% palladium-carbon. The mixture was stirred at 20 kg/cm2 hydrogen pressure for two days at room temperature. The mixture was then filtered, methyl alcohol was distilled off, the residue was dissolved in water, adjusted to pH 8 with saturated sodium bicarbonate, and extracted with ethyl acetate (100 ml×3). The ethyl acetate extracts were dried over magnesium sulfate, filtered, evaporated. The residue was dissolved in ethanol (50 ml) and a 1N hydrochloric acid (50 ml) was added thereto. The mixture was stirred for 1 h, the solvent was distilled off and the resultant solid were recrystallized from ethanol to give Fingolimod hydrochloride.

1. filtrationThe mixture was then filtered
2. distillationmethyl alcohol was distilled off
3. dissolutionthe residue was dissolved in water
4. extractionextracted with ethyl acetate (100 ml×3)
5. dry with materialThe ethyl acetate extracts were dried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. dissolutionThe residue was dissolved in ethanol (50 ml)
9. additiona 1N hydrochloric acid (50 ml) was added
10. distillationthe solvent was distilled off
11. customthe resultant solid were recrystallized from ethanol