Acetic Acid → 2-Amino-6-iodopurine

To a 2 liter single-neck round bottom flask with a mechanical stirrer was charged 2-amino-6-chloropurine (41.0 g, 242 mmol). The flask was cooled in an ice-water bath. The the reaction flask was charged HI (47% solution, pre-cooled in a refrigerator, 250 mL) in one portion. The resulting suspension was stirred for 16 hours at ice-water bath temperature. Water (500 mL) was charged to the reaction flask. The suspension was stirred at 0° C. for 1 hour. The precipitate was filtered and washed with water (3×250 mL). The filter cake was transferred to a 250 mL filtration flask. 6 M NaOH solution (85 mL) was added to the solid through the filter to rinse out residual solid and wash into the filter flask. The solution obtained was added slowly to a boiling solution of acetic acid (25 mL) and water (250 mL). The resulting suspension was cooled to room temperature and stirred at room temperature for 2 hours. The solid was collected by centrifugation, washed with water (2×250 mL), followed by heptane (250 mL). The solid was first spin-dried on the centrifuge for 30 minutes and then dried in a vacuum oven overnight to provide the desired product (61.3 g).

1. temperatureThe flask was cooled in an ice-water bath
2. temperaturepre-cooled in a refrigerator, 250 mL) in one portion
3. stirringThe suspension was stirred at 0° C. for 1 hour
4. filtrationThe precipitate was filtered
5. washwashed with water (3×250 mL)
6. filtrationThe filter cake was transferred to a 250 mL filtration flask
7. addition6 M NaOH solution (85 mL) was added to the solid through the
8. filtrationfilter
9. washto rinse out residual solid
10. washwash into the filter flask
11. customThe solution obtained
12. stirringstirred at room temperature for 2 hours
13. customThe solid was collected by centrifugation
14. washwashed with water (2×250 mL)
15. customThe solid was first spin-dried on the centrifuge for 30 minutes
16. customdried in a vacuum oven overnight

ORD record

ord-572086db5472427f947dca31a62dd061

Source dataset

uspto-grants-2003_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06613936B1