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To stirred, cooled concentrated sulfuric acid (40 ml) was added in portions 2,6-dichloro-4-methylbenzonitrile (13.2 g, 71.0 mmol). The mixture was heated on a steam bath for 3 hours with occasional shaking, cooled, poured into ice-water, and extracted twice with dichloromethane. The combined extracts were washed with brine, dried over anhydrous magnesium sulfate, and evaporated under vacuum. The residue was chromatographed on a column of silica gel (390 g) eluted with 4:1 (v/v) dichloromethane-diethyl ether to provide 8.6 g (59%) of 2,6-dichloro-4-methylbenzamide, m.p. 101°-107° C.

1. temperatureThe mixture was heated on a steam bath for 3 hours with occasional shaking
2. temperaturecooled
3. extractionextracted twice with dichloromethane
4. washThe combined extracts were washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated under vacuum
7. customThe residue was chromatographed on a column of silica gel (390 g)
8. washeluted with 4:1 (v/v) dichloromethane-diethyl ether