反应详情

温度

22.5 °C

A solution of 40 g of 2,3-dichlorobenzaldehyde (compound IX) in 160 mL of concentrated sulfuric acid (95-98% w/w) is heated to 40° C. and stirred to form a solution, then cooled to 20-25° C. Concentrated nitric acid (69-71% w/w; 24.7 g) is added to this solution over 20 minutes (an ice bath is used to maintain a reaction temperature of 20-30° C.). The reaction mixture is stirred at room temperature for 1 hour, and then added in portions to 600 mL of water. The resulting suspension is stirred for 2 hours and filtered. The filter cake is washed (3×50 mL of water). The filter cake is agitated with 200 mL of water for 2 hours and filtered. The filter cake is washed (3×50 mL of water) and dried in vacuo to give a mixture of the compound X and the isomer, 2,3-dichloro-5-nitrobenzaldehyde.

1. customto form a solution
2. temperatureto maintain a reaction temperature of 20-30° C.)
3. stirringThe reaction mixture is stirred at room temperature for 1 hour
4. stirringThe resulting suspension is stirred for 2 hours
5. filtrationfiltered
6. washThe filter cake is washed (3×50 mL of water)
7. stirringThe filter cake is agitated with 200 mL of water for 2 hours
8. filtrationfiltered
9. washThe filter cake is washed (3×50 mL of water)
10. customdried in vacuo
11. customto give