Diethyl o-nitrobenzoylmalonate

To the crude diethyl o-nitrobenzoylmalonate is added a solution of 60 ml. of glacial acetic acid, 7.6 ml. of concentrated sulfuric acid, and 40 ml. of water, and the mixture is heated under reflux for 4 hours (Note 4) or until no more carbon dioxide is evolved. The reaction mixture is chilled in an ice bath, made alkaline with 20% sodium hydroxide solution, and extracted with several portions of ether. The combined ethereal extracts are washed with water and dried with anhydrous sodium sulfate followed by Drierite, and the solvent is removed by distillation. On fractional distillation of the residue, 27.0-27.4 g. (82-83%) of light-yellow o-nitroacetophenone boiling at 158-159°/16 mm. is obtained n 1.548, wg 1.551, df 1.236) (Note 5). 

Diethyl methylphosphonate, 31, 34 Diethyl o-nitrobenzoylmalonate, 30, 71 Diethyl oxalate, 34, 13 Diethyl co-phthalimidobutylmalonate, 32, 15... 

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