Aluminum(III) Chloride → HCID 23303967, compound

HRID 1953238Notes

Reaction equation

HRID 1953238 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-d63bceb71a9c4a16885904d5f3bd0724
Source dataset
uspto-grants-2000_09
Patent number
US06114590

Reaction notes

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