反应详情

温度

5 °C

5-Amino-2,3-dichloropyridine (20.0 g, 123 mmol) was dissolved in 600 ml conc. HCl, and the solution cooled to 5° C. Sodium nitrate (8.5 g, 123 mmol) in 75 ml water was added dropwise, below the surface of the reaction, at such a rate that the temperature was maintained below 10° C. The reaction was stirred 15 minutes after the addition was complete. This mixture was then added rapidly to a solution of 600 ml acetic acid saturated with sulfur dioxide and containing also cupric chloride dihydrate (1.5 g), the solution cooled to 5° C. The reaction PG,38 was stirred at 5° C. for 20 minutes, then room temperature for 30 minutes and finally poured into 12 liters ice/water. The resulting solids were filtered off, washed with water, and air-dried. Yield: 17.27 g, 57 percent, m.p. 48°-51° C.

1. temperatureat such a rate that the temperature was maintained below 10° C
2. additionafter the addition
3. temperaturethe solution cooled to 5° C
4. customThe reaction PG,38
5. stirringwas stirred at 5° C. for 20 minutes
6. waitroom temperature for 30 minutes
7. filtrationThe resulting solids were filtered off
8. washwashed with water
9. customair-dried