Hydrogen iodide → 2-Amino-6-iodopurine

Participants

Reaction Conditions

Reaction Steps

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)

Provenance & Evidence