Carbon Dioxide → HCID 69801495, compound

Participants

Reaction Steps

245 g (2.4 mol) of malonic acid were dissolved in 360 ml of pyridine (exothermic, temperature raised to about 50° C.). Then 503 g of the crude benzyl 4-formylbenzoate obtained in step a) and 20 ml of piperidine were added, and the mixture was heated to reflux until the production of carbon dioxide had ceased (about 7 h). The mixture was cooled to room temperature, then 2 l of water were added and the product was precipitated by acidification of the stirred mixture with ca. 600 ml of concentrated hydrochloric acid to pH 1.8 at 10° C. The precipitated product was filtered off, washed with water and dried at 50° C. under reduced pressure. Combined yield of step a) and step b): 529.1 g (97%).

Provenance & Evidence