反应详情

To a mixture of 1,3-di-n-butyl-6-amino-uracil g, 112.8 mmol), glacial acetic acid (10 ml), and 6N HCl (18.8 ml) in water (500 ml) was added dropwise a solution of sodium nitrite (7.78, g, 112.8 mmol) in water (30 ml) on ice bath. The reaction mixture was stirred for 30 min. The violet solid was collected by filtration and washed with water (2×20 ml), dried for 2 days at 60° C. in a vacuum oven to yield 6-amino-1,3-di-n-butyl-5-nitroso-uracil (24.99 g, 82.6%), m.p. 199°-205° C.; 1H NMR (CDCl3) δ0.97-1.01 (m, 6H, 2×CH3), 1.36-1.49 (m, 4H, 2×CH2), 1.62-1.74 (m, 4H, 2×CH2), 3.94 (t, J=7.8 Hz, 2H, N--CH2), 4.08 (t, J=7.5 Hz, 2H, N--CH2), 6.46 (br s, 2H, NH2). Anal. Calc'd for C12H20N4O3 : C, 53.72; H, 7.51; N, 20.88; Found: C, 54.37; H, 7.67; N, 20.65.

1. filtrationThe violet solid was collected by filtration
2. washwashed with water (2×20 ml)
3. customdried for 2 days at 60° C. in a vacuum oven