反应详情

温度

27.5 °C

A 250 ml 4 neck round bottom flask equipped with mechanical stirrer, Thermo pocket was charged with DM water (15 ml) and 5,8,14-Triazatetracyclo[10.3.1.02,11.04,9]hexadeca-2(11),3,5,7,9-pentaene Tosylate salt (5 g, having a total purity of 99.71%). The above suspension was stirred for 30 min at 25-30° C. To this was added 8% aqueous sodium bicarbonate solution (150 ml) to adjust the pH to 8.0-9.0 at 25-30° C. MDC (30 ml) was added to this solution. The resulting mixture was stirred for 30 minutes at 20-25° C. The organic layer was separated, and the aqueous layer was extracted with MDC (4×30 ml). The combined organic layer was washed with DM water (30 ml). The organic layer was treated with activated Carbon (1.0 g), and stirred for 30 minutes at 25-30° C. The resulting solution was filtered through celite. Concentration afforded a solid product i.e. 5,8,14-Triazatetracyclo[10.3.1.02,11.04,9]hexadeca-2(11),3,5,7,9-pentaene. (Yield—2.5 g (95.06% (relative to VRN-Tosylate)), HPLC purity—99.65%).

1. customat 25-30° C
2. additionMDC (30 ml) was added to this solution
3. stirringThe resulting mixture was stirred for 30 minutes at 20-25° C
4. customThe organic layer was separated
5. extractionthe aqueous layer was extracted with MDC (4×30 ml)
6. washThe combined organic layer was washed with DM water (30 ml)
7. additionThe organic layer was treated with activated Carbon (1.0 g)
8. stirringstirred for 30 minutes at 25-30° C
9. filtrationThe resulting solution was filtered through celite
10. concentrationConcentration