Pivalic acid → HCID 178447533, compound

HRID 1108546Notes

Reaction equation

HRID 1108546 reaction equation
[Cl-].[Cl-].[CH2:3]([C:7]1([Hf+2:12]C2(CCCC)C=CC=C2)[CH:11]=[CH:10][CH:9]=[CH:8]1)[CH2:4][CH2:5][CH3:6].[C:22]([OH:28])(=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24].C(N(CC)CC)C>C1(C)C=CC=CC=1>[C:22]([O-:28])(=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24].[C:22]([O-:28])(=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24].[C:22]([O-:28])(=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24].[CH2:3]([C:7]1([Hf+3:12])[CH:11]=[CH:10][CH:9]=[CH:8]1)[CH2:4][CH2:5][CH3:6]

Participants

5

Reactant 3

HCID 6417Pivalic acidHCID 8471TriethylamineHCID 178441428HCID 178441428, compound

Product 1

HCID 178447533HCID 178447533, compoundYield 66%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To a solution of bis(n-butylcyclopentadienyl)hafnium dichloride (0.500 g, 1.012 mmol ) and pivalic acid (0.330 g, 3.230 mmol ) in toluene (30 ml) at 50° C. was added triethylamine (0.363 g, 3.240 mmol ) with stirring. A white precipitate formed immediately which was removed by filtration. The title compound was isolated as a dark yellow oil in 66% yield by evaporating the solvent under vacuum. The title compound such prepared exhibit purity above 95% based on NMR results. 1H NMR (toluene-d8) δ 6.15 (m, 2H), 5.90 (m,2H), 2.67 (t,J=7.6 Hz, 2H), 1.54 (m, 2H), 1.31 (m, 2H), 1.13 (s, 27H), 0.88 (t, J=7.2 Hz, 3H).

Workup

  1. customA white precipitate formed immediately which
  2. customwas removed by filtration

Sources & evidence

ORD record
ord-a6233a16a2454e57b23f5b8ee9fdc39a
Source dataset
uspto-grants-2000_05
Patent number
US06069109

Reaction notes

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