Triethylamine → 3-Oxo-butyric acid 4-cyclohexylpiperazide

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Reaction Steps

24 g (0.1 mol) of 1-cyclohexylpiperazine are suspended in 150 ml of absolute tetrahydrofuran. 20 ml of triethylamine are poured in and, after 20 minutes, 18.6 g of diketene in 20 ml of tetrahydrofuran are added dropwise, and the mixture is then stirred at room temperature for 2 h. Thereafter part of the solvent is removed by distillation in vacuo, the mixture is poured onto 200 ml of ice-water, 20 g of Na2CO3 are added, and extraction is carried out 3 times with 50 ml of methylene chloride each time. After the organic phase has been dried with MgSO4, crude 3-oxo-butyric acid 4-cyclohexylpiperazide is obtained as the residue from evaporation.

Provenance & Evidence