反应详情

温度

100 °C

A flask was charged with 4,6-dichloro-2-(propylthio)pyrimidin-5-amine (5 g), 2-(((3aR,4S,6R,6aS)-6-amino-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol L-tartaric acid salt (8.5 g), water (15 mL) and sodium bicarbonate (10.6 g). The mixture was heated to about 100° C. and maintained at the same temperature for about 20 hours and completion of the reaction was monitored by TLC. After completion of reaction the mixture was cooled to 30° C. followed by addition of water (50 mL) and ethyl acetate (25 mL). The mixture was stirred for about 10 minutes and layers were separated. The aqueous layer was extracted with ethyl acetate (25 mL). Total organic layer was washed with water (50 mL). The organic layer was subjected to complete distillation under vacuum at 55° C. followed by addition of ethyl acetate (5 mL). The mixture was stirred for 20 minutes followed by addition of n-hexane (75 mL). The mixture was further stirred at room temperature for solid separation followed by isolation of solid by filtration and washing with n-hexane (10 mL). The solid isolated was subjected to drying under vacuum at 60° C. for 3 hours to afford the title compound in about 91% yield having HPLC purity of about 99.18%.

1. temperaturemaintained at the same temperature for about 20 hours
2. customAfter completion of reaction the mixture
3. temperaturewas cooled to 30° C.
4. customlayers were separated
5. extractionThe aqueous layer was extracted with ethyl acetate (25 mL)
6. washTotal organic layer was washed with water (50 mL)
7. distillationThe organic layer was subjected to complete distillation under vacuum at 55° C.
8. additionfollowed by addition of ethyl acetate (5 mL)
9. stirringThe mixture was stirred for 20 minutes
10. additionfollowed by addition of n-hexane (75 mL)
11. stirringThe mixture was further stirred at room temperature for solid separation
12. filtrationfollowed by isolation of solid by filtration
13. washwashing with n-hexane (10 mL)
14. customThe solid isolated
15. customto drying under vacuum at 60° C. for 3 hours