Hydrogen Bromide → Bis(pentafluoroethyl)phosphinous acid

HRID 241313Notes

Reaction equation

HRID 241313 reaction equation
[OH-:1].[Na+].[F:3][C:4]([P:10](C(F)(F)C(F)(F)F)[C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])([F:9])[C:5]([F:8])([F:7])[F:6].Br>C(OCC)C>[F:3][C:4]([P:10]([C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])[OH:1])([F:9])[C:5]([F:8])([F:7])[F:6]

Participants

5

Procedure

29 mmol of a 1.5 molar aqueous sodium hydroxide solution are added to a solution of 5.2 g (13.3 mmol) of tris(pentafluoroethyl)phosphine in 50 ml of diethyl ether, and the mixture is stirred at room temperature for 15 minutes. After removal of the aqueous phase, 50 ml of 1,6-dibromohexane are added, and all volatile constituents are removed overnight in vacuo. The reaction mixture is reacted with 13 mmol of HBr, and the product is separated off from the reaction mixture by means of fractional condensation (3 cold traps at −30° C., −78° C. and −196° C.). The compound is stable at room temperature under inert-gas conditions.

Workup

  1. customAfter removal of the aqueous phase, 50 ml of 1,6-dibromohexane
  2. additionare added
  3. customall volatile constituents are removed overnight in vacuo
  4. customthe product is separated off from the reaction mixture by means of fractional condensation (3 cold traps at −30° C., −78° C. and −196° C.)
  5. customis stable at room temperature under inert-gas conditions

Sources & evidence

ORD record
ord-b037f0e295984bf58624b1db93da7871
Source dataset
uspto-grants-2014_02
Patent number
US08648202B2

Reaction notes

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