2-Phenylbutyric Acid → HCID 178454626, compound

HRID 1581464Notes

Reaction equation

HRID 1581464 reaction equation
[Cl-:1].[Cl-].[Cl-].[Cl-].[Hf+4:5].[C:6]1([CH:12]([CH2:16][CH3:17])[C:13]([OH:15])=[O:14])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>C1(C)C=CC=CC=1.[Hf]>[C:6]1([CH:12]([CH2:16][CH3:17])[C:13]([O-:15])=[O:14])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cl-:1].[Hf+2:5]

Participants

5

Reactant 2

HCID 70122-Phenylbutyric AcidHCID 9927068Hafnium chloride (HfCl4) (6CI,8CI); Hafnium chloride; Hafnium tetrachloride; Hafnium(IV) chloride; Hafnium chloride (HfCl4), (T-4)-

Product 1

HCID 178454626HCID 178454626, compound

Reagents, catalysts & solvents 2

HCID 1140TolueneSolvent2×HCID 23986HafniumSolvent2×

Procedure

16.4 g (51.1 mmoles) of hafnium tetrachloride (HfCl4) are suspended in 200 ml of toluene in a stirred 500 ml reactor. 16.8 g (102.2 mmoles) of 2-phenylbutyric acid dissolved in 100 ml of toluene, with a molar ratio 2-phenylbutyric acid/HfCl4 of 2.0, are added, under stirring, to the suspension, kept at room temperature. At the end of the addition, nitrogen is bubbled in for 3 hours, at room temperature, to facilitate the removal of hydrochloric acid. After this period, the suspension is filtered while hot and a solution is obtained which shows the following analysis: Hf=812 mmoles/l, Cl=1476 mmoles/l, with an atomic ratio Cl/Hf of 1.8. The yield in hafnium in solution is equal to 95.1% with respect to the initial hafnium.

Workup

  1. additionare added
  2. customkept at room temperature
  3. additionAt the end of the addition, nitrogen
  4. customis bubbled in for 3 hours, at room temperature
  5. customthe removal of hydrochloric acid
  6. waitAfter this period
  7. filtrationthe suspension is filtered while hot and a solution
  8. customis obtained which

Sources & evidence

ORD record
ord-7b57680596204cc6a313b5ceb895f92d
Source dataset
uspto-grants-2004_05
Patent number
US06730627B1

Reaction notes

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