反应详情

To a solution of 29.6 g (0.1 mole) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanol in 250 ml of THF was added 20 ml of liquid phosgene, followed by 9 ml of pyridine. The mixture was stirred at ambient temperature for about 21 hours. White solid (water-soluble) was filtered off and the THF filtrate concentrated in vacuum to a residual oil, the intermediate chloroformate. Further purification of the chloroformate was accomplished by dissolving it in about 300 ml of 1-chlorobutane, washing the butyl chloride solution with 0.5 N HCl (twice), water and saturated brine, drying (MgSO4), filtration, and evaporation of the filtrate in vacuum to leave, as a residual oil, 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-2-yl)-2-butyl chloroformate.

1. filtrationWhite solid (water-soluble) was filtered off
2. concentrationthe THF filtrate concentrated in vacuum to a residual oil
3. customFurther purification of the chloroformate
4. dissolutionby dissolving it in about 300 ml of 1-chlorobutane
5. washwashing the butyl chloride solution with 0.5 N HCl (twice), water and saturated brine
6. customdrying
7. filtration(MgSO4), filtration, and evaporation of the filtrate in vacuum