反应详情

With reference to FIG. 1, and H-shaped tube equipped with a Dimroth condenser and a Dimroth condenser having an IBr withdrawing cock was attached to a 500-ml four-necked flask. Into the flask were placed 200 ml (747 mM) of perfluorooctyl iodide (PFOI) and 5.0 ml (97.1 mM) of bomine, and the mixture was heated at 150° to 155° C. and irradiated with a 500-W visible light lamp. After the reaction mixture started to reflux, 49.5 ml (972 mM) of bromine was added dropwise to the mixture at a rate of 0.2 ml/min over a period of about 4 hours. The resulting IBr was drawn off at a suitable time through the IBr withdrawing Dimroth condenser. The reaction was continued for 5 hours, and the reaction mixture was thereafter cooled and washed with a 5% aqueous solution (200 ml) of sodium hydroxide to obtain 344.9 g (92.5% in yield) of perfluorooctyl bromide.

1. customWith reference to FIG. 1, and H-shaped tube equipped with a Dimroth condenser
2. customwas attached to a 500-ml four-necked flask
3. temperaturethe mixture was heated at 150° to 155° C.
4. customirradiated with a 500-W visible light lamp
5. temperatureto reflux
6. temperaturethe reaction mixture was thereafter cooled
7. washwashed with a 5% aqueous solution (200 ml) of sodium hydroxide