反应详情

Powdered 4,6-dihydroxy-2-methylpyrimidine (9 g, 71 mmol) was dissolved in trifluoroacetic acid (54 mL). The reaction mixture was cooled in ice-water as nitric acid (4.3 mL) was added dropwise over a period of 30 minutes. During addition the internal temperature was maintained below 15° C. After the addition, the cooling was removed and the reaction stirred overnight. Water (50 mL) was added to the reaction mixture and the resulting solid was filtered and dried under vacuum to obtain 2-methyl-5-nitropyrimidine-4,6-diol (5.8 g). 1H NMR (400 MHz, DMSO-d6): δ 12.97 (br, 2H), 2.32 (s, 3H). MS (m/z) 172 (M+1).

1. additionwas added dropwise over a period of 30 minutes
2. additionDuring addition the internal temperature
3. temperaturewas maintained below 15° C
4. additionAfter the addition
5. customthe cooling was removed
6. additionWater (50 mL) was added to the reaction mixture
7. filtrationthe resulting solid was filtered
8. customdried under vacuum