反应详情

In another experiment, a slurry of 2-amino-4,6-dichloro-5-{[(dimethyl-amino)methylene]amino}-pyrimidine (Example 2, 25.0 g, 0.107 mol) in 1.5 M aqueous potassium phosphate buffer (300 mL, prepared as above) was gently refluxed for 4 hours. pH was maintained at 3.2 by addition of 85% phosphoric acid, as required, throughout this period. The precipitate was filtered, washed with water (3×10 mL), methanol (2×10 mL), and dried (50° C., 25 mm Hg) to give the title compound as an off-white powder (16.0 g, 72%) with purity identical to that of the characterized sample described above (elemental analysis and 1H-NMR).

1. waitas required, throughout this period
2. filtrationThe precipitate was filtered
3. washwashed with water (3×10 mL), methanol (2×10 mL)
4. customdried (50° C., 25 mm Hg)