反应详情

温度

75 °C

5 mmol of sodium 3-[1-(triphenylmethyl)imidazol-4-yl]propoxide in 10 ml of toluene containing 0.5 mmol of 15-Crown-5 and 5 mmol of (3-chloropropyl)cyclohexane are mixed and the mixture is stirred for 24 h at 75° C. The suspension is concentrated under vacuum, the product obtained is dissolved in diethyl ether, the solution is filtered and the residue washed with petroleum ether (40°-60° C.). The filtrate obtained is concentrated and maintained for 1 h at the boiling point in a 2N aqueous/alcohol (ethanol/water) hydrochloric acid solution. The ethanol is removed under a low vacuum and the precipitate is filtered under vacuum. The solution is basified, extracted with dichloromethane and the organic phase is concentrated. The title compound obtained is recrystallized in the hydrogenmaleate form from ethanol/diethyl ether.

1. concentrationThe suspension is concentrated under vacuum
2. customthe product obtained
3. filtrationthe solution is filtered
4. washthe residue washed with petroleum ether (40°-60° C.)
5. customThe filtrate obtained
6. concentrationis concentrated
7. temperaturemaintained for 1 h at the boiling point in a 2N aqueous/alcohol (ethanol/water) hydrochloric acid solution
8. customThe ethanol is removed under a low vacuum
9. filtrationthe precipitate is filtered under vacuum
10. extractionextracted with dichloromethane
11. concentrationthe organic phase is concentrated