反应详情

温度

30 °C

5N hydrochloric acid (72 ml) and 10% Pd—C(10 g) were added to a solution of 4-(4-(4-(4-(((3R,5R)-5-((1H-1,2,4-triazol-1-yl)methyl)-5-(2,4-difluorophenyl)tetrahydro furan-3-yl)methoxy)phenyl)piperazin-1-yl)phenyl)-1-((2S,3R)-2-(benzyloxy)pentan-3-yl)-1H-1,2,4-triazol-5(4H)-one compound of formula-21 (42 g) in methanol (420 ml). The reaction mixture was hydrogenated for 5 hours under a hydrogen gas pressure of 4-5 kg/cm2 at 50°. After completion of reaction, the catalyst was filtered off and washed with methanol. pH of the filtrate was adjusted to ˜7.0 using 4N sodium hydroxide. Water was added to the reaction mixture and stirred for 2 hours at 25-35° C. Filtered the separated solid and washed with water. The obtained solid was dissolved in acetone (320 ml) and stirred at reflux temperature for 30 minutes. Filtered the undissolved product and added water to the filtrate and stirred the reaction mixture for 4 hours at 25-35° C. Filtered the separated solid and washed with water. Further the solid was recrystallized from isopropyl alcohol to get the title compound. Purity by HPLC: 99.85%; Yield: 75.0%: Chiral purity by HPLC: 99.82%.

1. customat 50°
2. customAfter completion of reaction
3. filtrationthe catalyst was filtered off
4. washwashed with methanol
5. additionWater was added to the reaction mixture
6. filtrationFiltered the separated solid
7. washwashed with water
8. dissolutionThe obtained solid was dissolved in acetone (320 ml)
9. stirringstirred
10. temperatureat reflux temperature for 30 minutes
11. filtrationFiltered the undissolved product
12. additionadded water to the filtrate
13. stirringstirred the reaction mixture for 4 hours at 25-35° C
14. filtrationFiltered the separated solid
15. washwashed with water
16. customFurther the solid was recrystallized from isopropyl alcohol