Hydrochloric Acid → HCID 13627533, compound

HRID 1589617Notes

Reaction equation

HRID 1589617 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](Cl)(=[O:18])[C:15]([CH3:17])=[CH2:16].C(=O)([O-])[O-].[Ca+2].Cl>C1C=CC=CC=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:18])[C:15]([CH3:17])=[CH2:16]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 10112Calcium CarbonateHCID 13528Methacryloyl chlorideHCID 36133332,3,5,6-Tetrafluoro-4-hydroxybenzonitrile

Product 1

HCID 13627533HCID 13627533, compoundYield 63.9%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

In 30 ml of benzene, 3.0 g (0.0157 mol) of 4-cyano-2,3,5,6-tetrafluorophenol and 1.80 g (0.0173 mol) of methacrylic acid chloride were dissolved. The resultant solution, and 1.73 g (0.0173 mol) of calcium carbonate added thereto as a hydrogen chloride trapping agent were stirred under reflux for 32 hours. The resultant reaction mixture was cooled off and filtered to separate calcium carbonate. The filtrate was dried with magnesium sulfate and then evaporated with a rotary evaporator. Consequently, there was obtained 2.6 g of 4-cyano-2,3,5,6-tetrafluorophenyl methacrylate (yeild 63.9% and purity 95.4%). The analyses obtained of the novel substance for the determination of its chemical structure were the same as those of Example 2.

Workup

  1. temperatureunder reflux for 32 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 with a rotary evaporator

Sources & evidence

ORD record
ord-bb95f3264134436e971880920d32f9bb
Source dataset
uspto-grants-1986_02
Patent number
US04572805

Reaction notes

Loading…