反应详情

温度

50 °C

A solution of 26.3 g (0.1 mol) of 1-cyclohexyl-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pent-1-en-3-ol (Example 2) in 50 ml of dioxan was added dropwise to a suspension of 3 g of 80% strength sodium hydride in 100 ml of dioxan. When the addition had ended, the mixture was warmed to 50° C. for 1 hour. After cooling, 10.9 g (0.1 mol) of ethyl bromide were added dropwise and the reaction mixture was heated under reflux overnight. After cooling, 10 ml of methanol were added and the mixture was concentrated in a rotary evaporator. The residue was taken up in methylene chloride and the methylene chloride mixture was washed with water. After drying the organic phase over sodium sulphate, it was filtered and the filtrate was concentrated. The residue was distilled. 11.0 g (37.8% of theory) of 1-cyclohexyl-3-ethoxy-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pent-1-ene of boiling point 110° C./0.07 mm Hg were obtained.

1. additionWhen the addition
2. temperatureAfter cooling
3. temperaturethe reaction mixture was heated
4. temperatureunder reflux overnight
5. temperatureAfter cooling
6. concentrationthe mixture was concentrated in a rotary evaporator
7. washthe methylene chloride mixture was washed with water
8. dry with materialAfter drying the organic phase over sodium sulphate, it
9. filtrationwas filtered
10. concentrationthe filtrate was concentrated
11. distillationThe residue was distilled