Benzene → HCID 13627534, compound

HRID 1589619Notes

Reaction equation

HRID 1589619 reaction equation
[C:1]([C:3]1[C:8]([F:9])=[C:7]([F:10])[C:6]([OH:11])=[C:5]([F:12])[C:4]=1[F:13])#[N:2].[C:14](=[O:17])([O-])[O-].[Ca+2].Cl.[CH:20]1C=CC=C[CH:21]=1>>[C:14]([O:11][C:6]1[C:5]([F:12])=[C:4]([F:13])[C:3]([C:1]#[N:2])=[C:8]([F:9])[C:7]=1[F:10])(=[O:17])[CH:20]=[CH2:21]

Participants

5

Reactant 4

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 10112Calcium CarbonateHCID 36133332,3,5,6-Tetrafluoro-4-hydroxybenzonitrile

Product 1

HCID 13627534HCID 13627534, compoundYield 57.1%

Procedure

In 30 ml of benzene, 3.82 g (0.020 mol) of 4-cyano-2,3,5,6-tetrafluorophenol and 2.26 g (0.025 mol) of calcium carbonate added thereto as a hydrogen chloride trapping agent were stirred under reflux for 40 hours. The resultant reaction mixture was cooled off and filtered to separate calcium carbonate. The filtrate was dried with magnesium sulfate and then evaporated to dryness with a rotary evaporator. Consequently, there was obtained 2.8 g of 4-cyano-2,3, 5,6-tetrafluorophenyl acrylate (yield 57.1%, purity 95.8%). The analyses obtained of the novel substance for the determination of its chemical structure were the same as those of Example 5.

Workup

  1. temperatureunder reflux for 40 hours
  2. customThe resultant reaction mixture
  3. temperaturewas cooled off
  4. filtrationfiltered
  5. customto separate calcium carbonate
  6. dry with materialThe filtrate was dried with magnesium sulfate
  7. customevaporated to dryness with a rotary evaporator

Sources & evidence

ORD record
ord-1cac325459d943e8af594be5dcaab32f
Source dataset
uspto-grants-1986_02
Patent number
US04572805

Reaction notes

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