反应详情

温度

110 °C

230.0 g (0.54 mol) of difluorotris(pentafluoroethyl)phosphorane and 41.2 g (1.089 mol) of sodium borohydride were refluxed with vigorous stirring for 3 hours in a glass flask at a bath temperature of about 110° C. The reaction mixture was subsequently distilled under reduced pressure (2 kPa), and two fractions of the product were collected in cold traps at a temperature of −78° C. and −195° C. respectively. For further purification, the combined products from both traps were distilled under atmospheric pressure under an inert-gas atmosphere, with the fraction in the boiling range 85-87° C. being collected. 194.0 g of pure tris(pentafluoroethyl)phosphine were obtained. The yield was 93%, based on the amount of difluorotris(pentafluoroethyl)phosphorane employed. The resultant product was characterised by means of 19F- and 31P-NMR spectroscopy. The chemical shifts found correspond to those from Example 1a.

1. distillationThe reaction mixture was subsequently distilled under reduced pressure (2 kPa), and two fractions of the product
2. customwere collected in cold traps at a temperature of −78° C. and −195° C. respectively
3. customFor further purification
4. distillationthe combined products from both traps were distilled under atmospheric pressure under an inert-gas atmosphere, with the fraction in the boiling range 85-87° C.
5. custombeing collected