反应详情

To a solution of 29.4 g (0.01 mole) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanone in 250 ml of THF was added 20 ml of liquid phosgene, followed by 9 ml of pyridine. After 3 days, the mixture was filtered and the filtrate evaporated in vacuum to a residual oil. The oil was dissolved in hot 1-chlorobutane and the solution filtered to remove a little white solid. The filtrate was cooled, precipitating a white solid. The solid was isolated by filtration, providing 12.9 g (36% of theoretical) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-1-buten-2-yl chloroformate, m.p. 159°-161°. The infrared spectrum showed absorption at ca 1800 cm-1.

1. filtrationthe mixture was filtered
2. customthe filtrate evaporated in vacuum to a residual oil
3. dissolutionThe oil was dissolved in hot 1-chlorobutane
4. filtrationthe solution filtered
5. customto remove a little white solid
6. temperatureThe filtrate was cooled
7. customprecipitating a white solid
8. customThe solid was isolated by filtration