反应详情

温度

27.5 °C

In a 3.0 lit 4 neck round bottom flask equipped with mechanical stirrer, Thermo pocket were charged DM water (507 ml) and 5,8,14-Triazatetracyclo[10.3.1.02,11.04,9]hexadeca-2(11),3,5,7,9-pentaene tosylate salt (169 g having a total purity of 99.99% obtained in example 6). The above suspension was stirred for 30 minutes at 25-30° C. To this was added 25% aqueous ammonia solution (60 ml) to adjust the pH to 9.0-10 at 25-30° C., and maintained with stirring for 30 minutes. MDC (507 ml) was charged in this solution. The resulting mixture was stirred for 30 minutes at 20-25° C. The layers were separated, and the aqueous layer was extracted with MDC (4×507 ml). The combined organic layer washed with DM water (507 ml). The organic layer was treated with activated Carbon (16.9 g), and stirred for 30 minutes at 25-30° C. The resulting solution was filtered through celite, concentrated to leave 1 volume of MDC with product, charged with 845 ml n-heptane at 45-50° C., and distilled under vacuum to remove a mixture of MDC and n-heptane to leave 3 volumes of n-heptane. The solid material was cooled to 25-30° C., and filtered at 25-30° C. to afford a solid product, i.e. 5,8,14-Triazatetracyclo[10.3.1.02,11.04,9]hexadeca-2(11),3,5,7,9-pentaene. The solid obtained was dried in vacuum oven at 45° to 50° C. (Yield—84 g (94.49% (relative to VRN-Tosylate)), HPLC purity—99.97%).

1. customIn a 3.0 lit 4 neck round bottom flask equipped with mechanical stirrer
2. customobtained in example 6)
3. customat 25-30° C.
4. temperaturemaintained
5. stirringwith stirring for 30 minutes
6. additionMDC (507 ml) was charged in this solution
7. stirringThe resulting mixture was stirred for 30 minutes at 20-25° C
8. customThe layers were separated
9. extractionthe aqueous layer was extracted with MDC (4×507 ml)
10. washThe combined organic layer washed with DM water (507 ml)
11. additionThe organic layer was treated with activated Carbon (16.9 g)
12. stirringstirred for 30 minutes at 25-30° C
13. filtrationThe resulting solution was filtered through celite
14. concentrationconcentrated
15. customto leave 1 volume of MDC with product
16. distillationdistilled under vacuum
17. customto remove
18. additiona mixture of MDC and n-heptane
19. customto leave 3 volumes of n-heptane
20. temperatureThe solid material was cooled to 25-30° C.
21. filtrationfiltered at 25-30° C.