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温度

0 °C

To a mixture of 2-chloro-3,5-dinitropyridine (2.035 g, 10 mmol) in EtOH (15 mL) was added aq. NH4OH (6 mL) dropwise at room temperature with stirring over 20 min. The resulting mixture was stirred at room temperature for 15 min, then cooled to 0° C. The precipitate was filtered, washed with water (3×5 mL) and dried to give 1.64 g (89%) of 61 as a yellow powder, mp 190°-1° C. (lit. 190°-2° C., Chemical Abstracts 63:14876 (1965)). 1H NMR (DMSO-d6): 8.697 (bs, 1H, D2O exchange), 8.947 (d, 1H, J=2.5), 9.164 (d, 1H, J=2.5), 9.224 (bs, 1H, D2O exchange).

1. stirringThe resulting mixture was stirred at room temperature for 15 min
2. filtrationThe precipitate was filtered
3. washwashed with water (3×5 mL)
4. customdried