Method for preparing fingolimod hydrochloride
A technology of fingolimod hydrochloride and preparation process, applied in the field of pharmaceutical synthesis, can solve the problems of low yield, unsuitable for large-scale production, long reaction time for hydroxyl and nitro groups, etc., achieves high total yield and shortens production The effect of simple cycle and post-reaction treatment
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0040] Preparation of compound (III). Add 200g of raw material compound (II), 800ml of absolute ethanol, add 160g of sodium ethoxide to a 2L flask, install a thermometer and reflux condenser, stir and heat to 50-55°C, stir and react for 5 hours, TLC detects that the reaction is complete, cool, The reaction solution was poured into 1L saturated sodium chloride solution, 800ml ethyl acetate was added, the layers were separated, and the organic phase was evaporated to dryness under reduced pressure to obtain 160g of crude light yellow oil compound (III). The crude product was directly carried out without further purification. One step response.
Embodiment 2
[0042] Preparation of compound (III). Add 100g of raw material compound (II), 600ml of anhydrous methanol to a 2L flask, add 130g of sodium methoxide, install a thermometer and reflux condenser, stir and heat to 60-65°C, stir and react for 8 hours, TLC detects that the reaction is complete, cool, The reaction solution was poured into 500 mL of saturated sodium chloride solution, 400 mL of ethyl acetate was added, the layers were separated, and the organic phase was evaporated to dryness under reduced pressure to obtain 76 g of crude light yellow oily compound (III). The crude product was carried out without further purification. One step response.
Embodiment 3
[0044] Preparation of compound (IV). Add 160g of compound (III) crude product, 900ml of dichloromethane to a 2L flask, install a thermometer and reflux condenser, add 220g of thionyl chloride in batches, after the addition, stir and heat to 80-85℃, stir and react for 2 h, TLC detects that the reaction is complete, cool, pour the reaction solution into 2L saturated ammonium chloride solution, stir and separate the liquids, and the organic phase is evaporated to dryness under reduced pressure to obtain 190 g of crude yellow oily compound (IV). The crude product is carried out without further purification. Next reaction.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More