反应详情

温度

95 °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 (30 mL) and sodium bicarbonate (10.5 g). The mixture was heated to about 90-100° C. and maintained at the same temperature for about 8-9 hours and completion of the reaction was monitored by TLC. After completion of reaction the mixture was cooled to 25-30° C. followed by addition of water (100 mL) and toluene (50 mL). The mixture was stirred for about 20 minutes and layers were separated. The organic layer was washed with water (50 mL). The organic layer was separated and subjected to complete distillation under vacuum at 60-65° C. followed by cooling to room temperature and subsequent addition of n-heptane (75 mL). The mixture was stirred for about 2 hours followed by isolation of solid by filtration and washing with n-heptane (10 mL). The solid isolated was subjected to drying under vacuum at 60-65° C. for 1 hour to afford the title compound in about 80% yield having HPLC purity of about 99.03%.

1. temperaturemaintained at the same temperature for about 8-9 hours
2. customAfter completion of reaction the mixture
3. temperaturewas cooled to 25-30° C.
4. customlayers were separated
5. washThe organic layer was washed with water (50 mL)
6. customThe organic layer was separated
7. distillationsubjected to complete distillation under vacuum at 60-65° C.
8. temperatureby cooling to room temperature
9. additionsubsequent addition of n-heptane (75 mL)
10. stirringThe mixture was stirred for about 2 hours
11. filtrationfollowed by isolation of solid by filtration
12. washwashing with n-heptane (10 mL)
13. customThe solid isolated
14. customto drying under vacuum at 60-65° C. for 1 hour