Бис (2,2,2-трифторэтил) фосф

Ссылки на синтез

Synthesis, p. 410, 1984 DOI: 10.1055/s-1984-30856

Синтез

The synthesis method of Bis(2,2,2-trifluoroethyl) Phosphite is as follows: A solution of phosphorus trichloride (43.5 mL, 0.50 mol) in dichloromethane (100 mL) was placed in an oven dried 1L round bottom flask. A reflux condenser and pressure equalizing addition funnel were attached to the round bottom flask. The addition funnel was charged with a solution of 2-methyl-2-propanol (48.0 mL, 0.50 mol) in dichloromethane (100 mL), and then the contents of the addition funnel were added in a dropwise manner to the round bottom flask under argon gas at 0 ℃over the course of 30 min. The reaction mixture was allowed to stir for an additional 30 min, then the addition funnel is recharged with a solution of 2,2,2-trifluoroethanol (70.0 mL, 0.96 mol) and dichloromethane (100 mL) and then the contents of the addition funnel were added in a dropwise manner to the round bottom flask under argon gas at 0 ℃ over the course of 30 min. The reaction mixture was then allowed to stir at RT overnight. The gaseous vapors were then degassed into NaOH (30.2 g, 0.98 mol) in 200 mL of water over the course of 8 hrs. The solvents were removed by rotary evaporation and the crude material was fractionally distilled under reduced pressure yielding Bis(2,2,2-trifluoroethyl) Phosphite (100.89 g, 0.41 mol, 82.2%) as colorless liquid.