Ethyl Acetoacetate → HCID 12333358, compound

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Reaction Steps

231.2 g (2.0 mol) of cyclohexan-1,3-dione (97%) are refluxed under nitrogen for 2.5 hours in 670 ml of absolute pyridine with 325.3 q (1.25×2.0 mol) of ethyl acetoacetate and 4.88 (0.02×2 mol) of 4-dimethylaminopyridine. Then 65.1 g (0.25×2.0 mol) of ethyl acetoacetate are again added and the mixture is boiled for a further 3 hours. The pyridine is then distilled off in vacuo and the oily residue is stirred while still warm with 100 ml of a mixture of cyclohexane/ethyl acetate (1:1). The reaction product which crystallises out is suction filtered and dried. Yield: 136.9 g (39.2% of theory) The mother liquor is freed from solvent in vacuo using a rotary evaporator and the oily residue is distilled in vacuo. The distillate solidifies into a white crystalline substance.

Provenance & Evidence