Benzene →

HRID 1578466Notes

Reaction equation

HRID 1578466 reaction equation
[Cl:1](F)(=[O:4])(=[O:3])=[O:2].[Cl-].[Cl-].[Cl-].[Al+3].[F-].[CH:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>>[Cl:1]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)(=[O:4])(=[O:3])=[O:2]

Participants

3

Procedure

225 grams (2.2 moles) of perchloryl fluoride gas was passed into a stirred suspension of 293 grams (2.2 moles) of aluminum trichloride in 4 liters of benzene at 10°-20°. The reaction was exothermic and the temperature was maintained within the desired limits by controlling the rate at which the fluoride was added and by cooling. By-product hydrogen chloride was removed as it formed. After about 3.5 hours, the amorphous aluminum salt was filtered from the reaction mixture. The filtrate was washed well with water, dried and the benzene was evaporated under reduced pressure (25 torr., 65°) in a dropping film rotary evaporator to give 258 grams (78% yield) of I, as a light yellow liquid.

Workup

  1. temperaturethe temperature was maintained within the desired limits
  2. additionwas added
  3. temperatureby cooling
  4. customBy-product hydrogen chloride was removed as it
  5. customformed
  6. filtrationthe amorphous aluminum salt was filtered from the reaction mixture
  7. washThe filtrate was washed well with water
  8. customdried
  9. customthe benzene was evaporated under reduced pressure (25 torr., 65°) in a dropping film rotary evaporator

Sources & evidence

ORD record
ord-13375478fbf049a9b4a046d320f5b8be
Source dataset
uspto-grants-1976_02
Patent number
US03937627

Reaction notes

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