反应详情

In accordance with K. von Werner, DE 39 25 525 Al (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. customvon Werner, DE 39 25 525 Al (1989), in a four-necked flask of 250 cm3 capacity, which is equipped with a dropping funnel (with bypass for pressure equalization), vane stirrer
2. temperaturethermometer and reflux condenser with superimposed check valve
3. additionis added drop by drop within one hour with vigorous stirring
4. temperaturewith refluxing for 9 hours
5. dissolutionhas dissolved
6. customThen the ether phase is separated
7. concentrationconcentrated with a rotary evaporator
8. customThe oily residue thus obtained
9. customThe solid product precipitated from the mixture
10. filtrationfiltered
11. customdried in the desiccator