The article describes analytical data (TLC, IR, MS) of 7-chloro-1-methyl-1,3-hydroxy-5-phenyl-2H-1,4-benzodiazepin-2-one (3-hydroxydiazepam) and 7-cyclopropyl-methyl-1,3-dihydro-3-hydroxy-5-phenyl-2H-1,4-benzodiazpin-2-one (3-hydroxy-prazepam). Analytical properties of important derivatives (N-oxides, 3-acetoxy compounds, re-arrangement products) are also reported. Besides preparation methods are given for the synthesis of these substances, considering in particular preparation as solution-reactions as well as reaction on the TLC-plate.