Perchloric Acid → HCID 18975193, compound

Participants

Reaction Steps

4.75 g (14.0 mmoles) of the isochromane derivative prepared in Step A are oxidized according to the method of Example 1, Step B using Jones' reagent with the exception that instead of reacting the crude product with perchloric acid, the 1-acetonyl-3,4-dichloro-4'-nitrobenzophenone derivative (m.p.: 121°-122° C.) is isolated by chromatography. The solution of the above derivative in isopropanol is reacted with 98% hydrazine hydrate at 25° C. to obtain the monohydrazone derivative (m.p.: 167°-169° C.). The monohydrazone compound is reacted with methanol containing 15% hydrogen chloride, then, the hydrochloride of the title compound is treated with triethylamine to obtain the free base that is purified by recrystallization from hot dimethylformamide. M.p.: 231°-233° C.

Provenance & Evidence