Aluminum(III) Chloride → HCID 23303967, compound

HRID 1421415Notes

Reaction equation

HRID 1421415 reaction equation
[Cl:1][C:2]1[C:3]([F:13])=[C:4]([C:9](F)(F)F)[CH:5]=[CH:6][C:7]=1[F:8].[Al+3].[Cl-:15].[Cl-:16].[Cl-:17]>C(Cl)Cl>[Cl:1][C:2]1[C:3]([F:13])=[C:4]([C:9]([Cl:17])([Cl:16])[Cl:15])[CH:5]=[CH:6][C:7]=1[F:8]

Participants

4

Reactant 2

HCID 6451240Aluminum(III) ChlorideHCID 143926222-Chloro-1,3-difluoro-4-(trifluoromethyl)benzene

Product 1

HCID 23303967HCID 23303967, compoundYield 86.9%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
42 °C

Procedure

216.5 g of 3-chloro-2,4-difluoro-benzotrifluoride in 440 ml of methylene chloride are initially introduced into a stirred apparatus, and 150 g of AlCl3 are introduced in small portions. The reaction is slightly exothermic. When the addition has ended, the mixture is heated under reflux (42° C.) for 2 hours, cooled and poured onto 1 l of ice-water. After intensive thorough mixing, the mixture is filtered over a suction filter and the organic phase is then separated off. After drying, the methylene chloride phase is distilled. 231 g of 3-chloro-2,4-difluoro-benzotrichloride with a boiling range of 124-126° C./18 mbar are obtained.

Workup

  1. additionare introduced in small portions
  2. additionWhen the addition
  3. temperaturethe mixture is heated
  4. temperaturecooled
  5. filtrationAfter intensive thorough mixing, the mixture is filtered over a suction
  6. filtrationfilter
  7. customthe organic phase is then separated off
  8. customAfter drying
  9. distillationthe methylene chloride phase is distilled

Sources & evidence

ORD record
ord-ada5d7286781454aa1537b3e74514479
Source dataset
uspto-grants-2000_06
Patent number
US06075165

Reaction notes

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