Hydrogen iodide → 2-Amino-6-iodopurine

Temperature

5 °C

Charge 57% Hydriodic acid (10.90 kg) into a suitable vessel under nitrogen and then the solution was cooled to 0 to 10° C. Then 2-amino-6-chloropurine (0.8 kg) was charged into the solution at about 15° C. After 2 h for the completion, water (8 kg) was slowly charged to the reaction mixture at r.t. and stirred for about 0.5 h. The yellow precipitate was filtered and washed with water. The wet cake was transferred to a suitable vessel, and water (2.0 kg) and 20% NaOH aqueous solution (0.4 kg) were slowly charged to dissolve the solids at r.t. Then THF (2.14 kg) was charged into the solution and 10% HOAc (4.8 kg) was slowly charged into the solution at about 35° C. to observe slurry mixture. The resultant slurry was stirred filtered and washed with acetone (3.8). The wet cake was dried under vacuum at 70° C. to afford SPT1255C1 (1.14 kg). Yield: 90-98%. 1H NMR (400 MHz, DMSO-d6) 6.65 (s, 2H, NH2), 8.04 (s, 1H, H8)

1. filtrationThe yellow precipitate was filtered
2. washwashed with water
3. customThe wet cake was transferred to a suitable vessel
4. additionwater (2.0 kg) and 20% NaOH aqueous solution (0.4 kg) were slowly charged
5. dissolutionto dissolve the solids at r.t
6. additionThen THF (2.14 kg) was charged into the solution and 10% HOAc (4.8 kg)
7. additionwas slowly charged into the solution at about 35° C.
8. stirringThe resultant slurry was stirred
9. filtrationfiltered
10. washwashed with acetone (3.8)
11. customThe wet cake was dried under vacuum at 70° C.
12. customto afford SPT1255C1 (1.14 kg)

ORD record

ord-72e4e8389fd24970913d13956dd80ecb

Source dataset

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08481728B2