Chlorotrifluoroethylene → HCID 14405126, compound

HRID 1903860Notes

Reaction equation

HRID 1903860 reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([OH:9])[C:5](=[CH:7][CH:8]=1)[OH:6].[OH-].[K+].[F:12][C:13]([F:17])=[C:14]([F:16])Cl>C1S(=O)(=O)CCC1>[CH3:1][C:2]1[CH:8]=[CH:7][C:5]2[O:6][C:13]([F:17])([F:12])[CH:14]([F:16])[O:9][C:4]=2[CH:3]=1

Participants

5

Reactant 3

HCID 6594ChlorotrifluoroethyleneHCID 99584-MethylcatecholHCID 14797Potassium Hydroxide

Product 1

HCID 14405126HCID 14405126, compound

Reagents, catalysts & solvents 1

HCID 31347SulfolaneSolvent

Procedure

124 g of 4-methylpyrocatechol were initially introduced into 300 ml of tetramethylene sulphone, together with 110 g of potassium hydroxide, at 110° C. 170 g of trifluorochloroethylene were then passed in in the course of 4 hours. The mixture was then distilled over a column under 15 mm Hg, the distillate being removed up to a transition temperature of 85° C. After separating off the aqueous phase in the receiver, the product was again distilled. 133 g ( 65% of theory) of 6-methyl-2,2,3-trifluoro-1,4-benzodioxene were obtained at a boiling point 70°-72° C./12 mm Hg (nD20 : 1.4565).

Workup

  1. customwere then passed in in the course of 4 hours
  2. distillationThe mixture was then distilled over a column under 15 mm Hg
  3. customthe distillate being removed up to a transition temperature of 85° C
  4. customAfter separating off the aqueous phase in the receiver
  5. distillationthe product was again distilled
  6. custom133 g ( 65% of theory) of 6-methyl-2,2,3-trifluoro-1,4-benzodioxene were obtained at a boiling point 70°-72° C./12 mm Hg (nD20 : 1.4565)

Sources & evidence

ORD record
ord-eb45545f58e249a789afd37932e59859
Source dataset
uspto-grants-1984_03
Patent number
US04438275

Reaction notes

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