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An efficient preparation of 7-chloro-l-methyl-3,4-dihydro-lfl-l,4-benzodiazepine-2,5-dione from 5-chloro-jVmethylisatoic anhydride and glycine has been devised, and from it, by the action of phenylmagnesium chloride on its N-acetyl derivative followed by treatment with hydroxylamine and cleavage of the resulting desacetyl oxime with sodium bisulfite, diazepam has been synthesized. The overall yield is about 50% from 5-chloroisatoic anhydride.