Phosphoric Acid → HCID 19090856, compound

HRID 2050734Notes

Reaction equation

HRID 2050734 reaction equation
P(=O)(O)(O)O.[I-:6].[F:7][C:8]([F:15])([F:14])[CH:9]([CH3:13])[CH2:10][CH2:11]O>>[F:7][C:8]([F:15])([F:14])[CH:9]([CH3:13])[CH2:10][CH2:11][I:6]

Participants

4

Reactant 3

HCID 1004Phosphoric AcidHCID 30165Iodide IonHCID 2743554,4,4-Trifluoro-3-methyl-1-butanol

Product 1

HCID 19090856HCID 19090856, compound

Procedure

To a mixture of 19 g phosphoric acid (98%) and 19 g pottasium iodide are added at 40° under stirring 4.75 g (33.4 mMol) of 4,4,4-trifluoro-3-methyl-butan-1-ol over a period of 10 minutes. The mixture is then heated at 120° for 16 hours, a cooling poured into ice-water and extracted with diethylether. The etheric extracts are washed with 10% sodium thiosulfate and brine acid dried over sodium sulphate. After filtration, the solvent is removed through a 15 cm Vigreux-column at atmospheric pressure, followed by fractionation giving 4,4,4-trifluoro-3-methyl-1-iodo-butane, b.p. 76-77° at 140 mbar.

Workup

  1. additionare added at 40°
  2. temperatureThe mixture is then heated at 120° for 16 hours
  3. extractionextracted with diethylether
  4. washThe etheric extracts are washed with 10% sodium thiosulfate and brine acid
  5. dry with materialdried over sodium sulphate
  6. filtrationAfter filtration
  7. customthe solvent is removed through a 15 cm Vigreux-column at atmospheric pressure

Sources & evidence

ORD record
ord-99adbbd40292421f97cb457941632286
Source dataset
uspto-grants-1991_05
Patent number
US05013863

Reaction notes

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