Potassium Carbonate → HCID 76818454, compound

Participants

Reaction Steps

N-Methylpiperazine (104.16 g, 1041.6 mmol, 1.0 eq.) was added dropwise to a solution of 2-cyclohexen-1-one (100.0 g, 1041.6 mmol, 1.0 eq.) in ethanol (300 ml), and the resulting mixture was stirred for 5 hours at RT. The reaction solution was diluted with ethanol (600 ml) and cooled to 0° C.; K2CO3 (172.48 g, 1249.9 mmol, 1.2 eq.) and NH2OH.HCl (86.7 g, 1249.9 mmol, 1.2 eq.) were added, and the mixture was stirred for 30 minutes at 0° C. and then heated to RT and stirred for a further 16 hours. The reaction mixture was filtered off over Celite and washed with ethanol (500 ml). The filtrate was concentrated under reduced pressure and the residue was taken up in THF (100 ml) and n-hexane (500 ml) and stirred for 3 hours. The resulting solid was filtered off and used in the next stage without being purified further. Yield: 54% (120.0 g, 568.7 mmol)

Provenance & Evidence