Bis(2,2,2-trifluoroethyl) phosphite was used in the synthesis of bis(2,2,2-trifluoroethyl phosphorochloridate. It was also employed as reagent for the synthesis of mono- and diesters of phosphorous acid.
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.
