反应详情

温度

0 °C

A mixture of 12.7 g (0.06 mole) of 1-(5-methyl-1,3-dioxan-5-yl)-2-(1,2,4-triazol-1-yl)-ethan-1-one, 10.8 g (0.06 mole) of 2,4-dichlorobenzaldehyde, 1 g of piperidine, 0.5 g of acetic acid and 150 ml of toluene is stirred for 10 hours under reflux, with elimination of water. The mixture is then cooled, washed with three times 80 ml of water, dried over sodium sulfate and concentrated under reduced pressure. The residue is dissolved in 250 ml of acetonitrile and the solution is decolorized with 1 g of animal charcoal at 40° C., concentrated to 40 ml and cooled to 0° C. The colorless precipitate is filtered off, washed with 40 ml of ether and dried. 18.4 g (83.3%) of 1-(5-methyl-1,3-dioxan-5-yl)-2-(1,2,4-triazol-1-yl)-3-(2,4-dichlorophenyl)-propen-1-one, of melting point 133°-135° C., are obtained.

1. temperatureThe mixture is then cooled
2. washwashed with three times 80 ml of water
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. dissolutionThe residue is dissolved in 250 ml of acetonitrile
6. customis decolorized with 1 g of animal charcoal at 40° C.
7. concentrationconcentrated to 40 ml
8. filtrationThe colorless precipitate is filtered off
9. washwashed with 40 ml of ether
10. customdried