反应详情

温度

27.5 °C

In a 250 ml 4 neck round bottom flask equipped with mechanical stirrer, Thermo pocket were charged DM water (30 ml) and 5,8,14-Triazatetracyclo[10.3.1.02,11.04,9]hexadeca-2(11),3,5,7,9-pentaene Tosylate salt (10 g, having a total purity of 99.42% obtained in example 4). The above suspension was stirred for 30 minutes at 25-30° C. To this was added 25% aqueous ammonia solution (5 ml) to adjust the pH to 9.0-10 at 25-30° C., and 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 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-5 g (95.06% (relative to VRN-Tosylate)), HPLC purity-99.43%).

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