反应详情

In accordance with K. von Werner, DE 39 25 525 A1 (1989), in a four-necked flask of 250 cm3 capacity, which is equipped with a dropping funnel (with bypass for pressure equalization), vane stirrer, thermometer and reflux condenser with superimposed check valve, 1.82 g (0.075 mol) magnesium chips are placed under argon in 10 cm3 of anhydrous di-n-propyl ether and activated with a few drops of methyl iodide with gentle heating. The temperature is raised to 80° C. while a mixture of 23.7 g (0.05 mol) of C6F13CH2CH2I and 60 cm3 of anhydrous di-n-propyl ether is added drop by drop within one hour with vigorous stirring. Then the mixture is stirred with refluxing for 9 hours and then cooled to 10° C., hydrolyzed with 100 cm3 of 5 wt.-% aqueous hydrochloric acid until the excess magnesium has dissolved. Then the ether phase is separated and concentrated with a rotary evaporator. The oily residue thus obtained is treated with 30 cm3 of chloroform and let stand for 1 hour at 0° C. The solid product precipitated from the mixture is suction filtered and dried in the desiccator. 11.0 g of C6F13(CH2)4C6F13 is obtained as nearly colorless crystals which have a melting point of 48° C. The yield is 63.2% of the theoretical.

1. temperaturethermometer and reflux condenser with superimposed check valve
2. additionis added drop by drop within one hour with vigorous stirring
3. temperaturewith refluxing for 9 hours
4. dissolutionhas dissolved
5. customThen the ether phase is separated
6. concentrationconcentrated with a rotary evaporator
7. customThe oily residue thus obtained
8. customThe solid product precipitated from the mixture
9. filtrationfiltered
10. customdried in the desiccator