反应详情

A solution of 838 mg (2.2 mmole) of 2-acetamido-9-(1,3-diacetoxy-2-propoxymethyl)hypoxanthine in 8.5 ml of 40% methylamine (aqueous) was stirred at gentle reflux under N2 for 1 hour. The solution was then cooled and concentrated to dryness. The residual white solid was recrystallized from a minimum volume of H2O containing 2 drops of acetic acid. After standing in the refrigerator, the product was collected on a filter and washed with a small amount of H2O, then acetone. The material was dried under high vacuum at 75° for 3 hours to giive 529 mg (90% based on hydration with 0.75H2O) of white crystals, mp 249°-250° dec. The material was homogeneous by TLC (80:20:2 CHCl3 --MeOH--H2O), and the structure was confirmed by NMR.

1. temperatureat gentle reflux under N2 for 1 hour
2. temperatureThe solution was then cooled
3. concentrationconcentrated to dryness
4. customThe residual white solid was recrystallized from a minimum volume of H2O containing 2 drops of acetic acid
5. customthe product was collected on
6. filtrationa filter
7. washwashed with a small amount of H2O
8. customThe material was dried under high vacuum at 75° for 3 hours to giive 529 mg (90% based on hydration with 0.75H2O) of white crystals, mp 249°-250° dec