tetrachloro(phenyl)-lambda5-phosphane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Variant b) The mixture of 4.6 g (18.4 mmol) of phenyltetrachlorophosphorane and 7.3 g (14.5 mmol) of bis(nonafluorobutyl)phosphinic acid is stirred at room temperature for four hours When the evolution of gas (HCl) is complete, the nonafluorobutylphosphonyl dichloride is separated off by distillation at atmospheric pressure, giving 5.73 g of bis(nonafluorobutyl)phosphinyl chloride as colourless liquid substance. This corresponds to a yield of 76%, based on the phosphinic acid employed. the nonafluorobutylphosphonyl dichloride is separated off by distillation at atmospheric pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Variant a) 2.49 g (5.0 mmol) of bis(nonafluorobutyl)phosphinic acid are added dropwise at room temperature to a solution of 1.47 g (5.9 mmol) of phenyltetrachlorophosphorane in 3 cm3 of dry chloroform, and the mixture is stirred for a further 50 minutes. Chloroform is separated off by distillation, and bis(nonafluorobutyl)phosphinyl chloride is distilled off at atmospheric pressure, giving 1.62 g of bis(nonafluorobutyl)phosphinyl chloride, which corresponds to a yield of 63%, based on the phosphinic acid employed. Chloroform is separated off by distillation, and bis(nonafluorobutyl)phosphinyl chloride is distilled off at atmospheric pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 21.75 g (72 mmol) of bis(pentafluoroethyl)phosphinic acid are added dropwise at room temperature to 20.0 g (80 mmol) of phenyltetrachlorophosphorane, and the mixture is stirred for four hours. Bis(pentafluoroethyl)phosphinyl chloride is separated off by distillation at atmospheric pressure, giving 18.1 g of bis(pentafluoroethyl)phosphinyl chloride, which corresponds to a yield of 78%, based on the phosphinic acid employed. Bis(pentafluoroethyl)phosphinyl chloride is separated off by distillation at atmospheric pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Variant b) The mixture of 4.6 g (18.4 mmol) of phenyltetrachlorophosphorane and 7.3 g (14.5 mmol) of bis(nonafluorobutyl)phosphinic acid is stirred at room temperature for four hours When the evolution of gas (HCl) is complete, the nonafluorobutylphosphonyl dichloride is separated off by distillation at atmospheric pressure, giving 5.73 g of bis(nonafluorobutyl)phosphinyl chloride as colourless liquid substance. This corresponds to a yield of 76%, based on the phosphinic acid employed. the nonafluorobutylphosphonyl dichloride is separated off by distillation at atmospheric pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Variant a) 2.49 g (5.0 mmol) of bis(nonafluorobutyl)phosphinic acid are added dropwise at room temperature to a solution of 1.47 g (5.9 mmol) of phenyltetrachlorophosphorane in 3 cm3 of dry chloroform, and the mixture is stirred for a further 50 minutes. Chloroform is separated off by distillation, and bis(nonafluorobutyl)phosphinyl chloride is distilled off at atmospheric pressure, giving 1.62 g of bis(nonafluorobutyl)phosphinyl chloride, which corresponds to a yield of 63%, based on the phosphinic acid employed. Chloroform is separated off by distillation, and bis(nonafluorobutyl)phosphinyl chloride is distilled off at atmospheric pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Variant a) 2.49 g (5.0 mmol) of bis(nonafluorobutyl)phosphinic acid are added dropwise at room temperature to a solution of 1.47 g (5.9 mmol) of phenyltetrachlorophosphorane in 3 cm3 of dry chloroform, and the mixture is stirred for a further 50 minutes. Chloroform is separated off by distillation, and bis(nonafluorobutyl)phosphinyl chloride is distilled off at atmospheric pressure, giving 1.62 g of bis(nonafluorobutyl)phosphinyl chloride, which corresponds to a yield of 63%, based on the phosphinic acid employed. Chloroform is separated off by distillation, and bis(nonafluorobutyl)phosphinyl chloride is distilled off at atmospheric pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 21.75 g (72 mmol) of bis(pentafluoroethyl)phosphinic acid are added dropwise at room temperature to 20.0 g (80 mmol) of phenyltetrachlorophosphorane, and the mixture is stirred for four hours. Bis(pentafluoroethyl)phosphinyl chloride is separated off by distillation at atmospheric pressure, giving 18.1 g of bis(pentafluoroethyl)phosphinyl chloride, which corresponds to a yield of 78%, based on the phosphinic acid employed. Bis(pentafluoroethyl)phosphinyl chloride is separated off by distillation at atmospheric pressure

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir: