Acetic Acid → 1-(4-Chlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-1-penten-3-one

Participants

Reaction Steps

167 g (1 mol) of 3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one and 140.5 g (1 mol) of 4-chlorobenzaldehyde were dissolved in 700 ml of toluene and 1.2 g (0.02 mol) of glacial acetic acid and 1.8 ml (0.02 mol) of piperidine were added. The reaction mixture was heated for 40 hours to 120° C., while continuously separating off the water of reaction. Thereafter the reaction mixture was concentrated in vacuo and the oil which remained was distilled (boiling range 130°-160° C./0.04 mm Hg). The distillate was stirred with ethanol, whereupon crystals separated out. These were filtered off and dried. 35 g (12% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pent-1-en-3-one (E isomer) of melting point 110° C. were thus obtained.

Provenance & Evidence