反应详情

Trans-4-(2-Amino-6-chloro-8-oxo-7,8-dihydropurin-9-yl)cyclohexyl methyl carbonate (1.43 g) was dissolved in 80 mL of an aqueous solution 0.5 N KOH and the reaction mixture heated at reflux for 30 min (LC-MS analysis indicated reaction to be complete). The reaction mixture was then cooled in an ice bath, and its pH was brought to 7 by drop wise addition of a concentrated aqueous solution of HCl. A light pink solid precipitated. It was filtered under vacuum, thoroughly dried in vacuum oven at 60° C., to give the desired product in 86% yield. 1H NMR (300 MHz, CDCl3+CD3OD) δ, ppm: 8.48 (br s, 1H), 7.73 (s, 2H), 4.26-4.18 (m, 1H), 3.70-3.61 (m, 1H), 2.53-2.40 (m, 2H), 2.10-2.06 (m, 2H), 1.81-1.76 (m, 2H), 1.48-1.37 (m, 2H); MS (EI) m/z 284.1 (MH)+.

1. temperaturethe reaction mixture heated
2. temperatureat reflux for 30 min
3. custom(LC-MS analysis indicated reaction to be complete)
4. temperatureThe reaction mixture was then cooled in an ice bath
5. customA light pink solid precipitated
6. filtrationIt was filtered under vacuum
7. customthoroughly dried in vacuum oven at 60° C.