Hydrochloric Acid → HCID 20131409, compound

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Reaction Steps

22.5 ml of 100% nitric acid are added dropwise at 20° C. within 30 min. to 20 g of the above compound in 200 ml of dichloromethane, and the mixture is stirred for a further 15 h at room temperature. Analogously to Example B7c, this gives N-(4-difluoromethoxy-5-fluoro-2-nitrophenyl)acetamide of m.p. 72°-74° C. (from cyclohexane) in 89% yield. By stirring for several hours with 1M hydrochloric acid in methanol at 60° C., 4-difluoromethoxy-5-fluoro-2-nitroaniline of m.p. 95°-97.5° C. is obtained in 95% yield and, analogously to Example B7e, 4-difluoromethoxy-5-fluoro-1,2-phenylenediamine dihydrochloride (decomposition from 210° C.) is obtained in 85% yield.

Provenance & Evidence