反应详情

温度

90 °C

A suspension of 60.3g (0.37 mole) 2,6-dichloro-3-aminopyridine and salicylic acid 61g (0.44 mole) in 300 mL of toluene were heated to reflux for one hour. The reaction mixture was cooled at 90° C. and 34.2 ml (0.47 mole) of thionyl chloride was slowly added. After the addition the reaction mixture was refluxed for 3 hours, then cooled to room temperature. To the reaction mixture was added a solution containing 20g NaOH in 740 mL of H2O. The organic phase was separated and washed with water. The organic phase was treated with charcoal, filtered and the filtrate treated with CO2, the brownish precipitate was filtered off. Recrystallization from isopropyl alcohol gave 63.3g (60.5%) mp 179°-186° C.

1. temperaturewere heated
2. temperatureto reflux for one hour
3. additionAfter the addition the reaction mixture
4. temperaturewas refluxed for 3 hours
5. temperaturecooled to room temperature
6. additionTo the reaction mixture was added a solution
7. customThe organic phase was separated
8. washwashed with water
9. additionThe organic phase was treated with charcoal
10. filtrationfiltered
11. additionthe filtrate treated with CO2
12. filtrationthe brownish precipitate was filtered off
13. customRecrystallization from isopropyl alcohol
14. customgave 63.3g (60.5%) mp 179°-186° C.