反应详情

温度

62.5 °C

Emtricitabine hydrochloride (100 g) was dissolved in methanol (500 ml). The mixture was stirred for 15 mins. Triethylamine (80 g) was added to the solution at 25-35° C. The solution was heated to reflux and maintained at reflux temperature 60-65° C. for 60 mins. The reaction mass was cooled to 25-35° C. and decolourised with activated carbon at 25-35° C. Filtrate was distilled under vacuum to thick residue below 50° C. The mass was cooled to 25-35° C. Traces of methanol was removed by flushing with methylene chloride (100 ml). Methylene chloride was charged to the residue and heated to reflux. Reaction mass was maintained at reflux temperature for 2 hrs. The suspension was cooled to 25° C. The reaction mass was maintained at 25-35° C. for 1 hr. Solid was collected by filtration and leached with methylene chloride (200 ml) and washed with methylene chloride (100 ml). The solid was dried at 45-50° C. to get Emtricitabine (67 gm, 82%). This technical grade Emtricitabine can be decolourised in IPA to get pharmaceutically accepted quality product

1. temperatureThe solution was heated
2. temperatureto reflux
3. temperaturemaintained
4. temperatureThe reaction mass was cooled to 25-35° C.
5. customdecolourised with activated carbon at 25-35° C
6. distillationFiltrate was distilled under vacuum to thick residue below 50° C
7. temperatureThe mass was cooled to 25-35° C
8. customTraces of methanol was removed
9. customby flushing with methylene chloride (100 ml)
10. additionMethylene chloride was charged to the residue
11. temperatureheated to reflux
12. customReaction mass
13. temperaturewas maintained
14. temperatureat reflux temperature for 2 hrs
15. temperatureThe suspension was cooled to 25° C
16. temperatureThe reaction mass was maintained at 25-35° C. for 1 hr
17. filtrationSolid was collected by filtration
18. washwashed with methylene chloride (100 ml)
19. customThe solid was dried at 45-50° C.