反应详情

温度

5 °C

A stirred 0° C. solution of 2,6-dichloro-4-methylbenzamide (8.6 g, 42. mmol) in 2:1 (v/v) acetic acid-concentrated hydrochloric acid (165 ml) was treated dropwise with a solution of sodium nitrite (19.0 g, 275 mmol) in water (42 ml). The mixture was stirred 30 minutes at 5° C., slowly warmed to 85° C., and kept 1 hour. The mixture was cooled, concentrated under vacuum, and treated with cold water (50 ml). The product was filtered, washed twice with cold water, and dried 16 hours at 50° C. over phosphorus pentoxide under vacuum to provide 7.15 g (83%) of 2,6-dichloro-4-methylbenzoic acid, m.p. 139°-145° C.

1. temperatureslowly warmed to 85° C.
2. waitkept 1 hour
3. temperatureThe mixture was cooled
4. concentrationconcentrated under vacuum
5. additiontreated with cold water (50 ml)
6. filtrationThe product was filtered
7. washwashed twice with cold water
8. dry with materialdried 16 hours at 50° C. over phosphorus pentoxide under vacuum