反应详情

13.7 g (0.1% mol) of p-chlorophenyl-acetylene are added to a mixture of 10.1 g (0.1 mol) of triethylamine, 1.4 g (0.01 mol) of copper(I) bromide and 55 ml of toluene, and the mixture is stirred for 30 minutes at room temperature under argon. After the reaction mixture has been heated to 55° C., 15.5 g (0.1 mol) of 1-methyl-2,2-difluoro-cyclopropanecarbonyl chloride are added dropwise. After this, the mixture is stirred for 8 hours at 90° C., and then cooled and filtered. The filtrate is washed in succession with dilute aqueous hydrochloric acid and water and concentrated under reduced pressure. 19.2 g of a dark oil remain, which is distilled using a bulb tube. At 0.1 mbar and a jacket temperature of 120° C., a yellow oil passes over which solidifies on standing. 8.4 g (33% of theory) of 2-(4-chlorophenyl)-ethin-1-yl 2,2-difluoro-1-methylcycloprop-1-yl ketone of melting point 67°-68° C. are obtained. ##STR65##

1. temperatureAfter the reaction mixture has been heated to 55° C.
2. stirringAfter this, the mixture is stirred for 8 hours at 90° C.
3. temperaturecooled
4. filtrationfiltered
5. washThe filtrate is washed in succession with dilute aqueous hydrochloric acid and water
6. concentrationconcentrated under reduced pressure
7. distillationwhich is distilled
8. customa jacket temperature of 120° C.