Pivalic acid → HCID 178447531, compound

HRID 1353016Notes

Reaction equation

HRID 1353016 reaction equation
[Cl-].[Cl-].[CH3:3][C:4]1[C:8]([Zr+2:10][C:11]2([CH3:20])[C:15]([CH3:16])=[C:14]([CH3:17])[C:13]([CH3:18])=[C:12]2[CH3:19])([CH3:9])[C:7]([CH3:21])=[C:6]([CH3:22])[C:5]=1[CH3:23].[C:24]([OH:30])(=[O:29])[C:25]([CH3:28])([CH3:27])[CH3:26].C(N(CC)CC)C>C1(C)C=CC=CC=1>[C:24]([O-:30])(=[O:29])[C:25]([CH3:28])([CH3:27])[CH3:26].[C:24]([O-:30])(=[O:29])[C:25]([CH3:28])([CH3:27])[CH3:26].[CH3:16][C:15]1[C:11]([Zr+2:10][C:8]2([CH3:9])[C:7]([CH3:21])=[C:6]([CH3:22])[C:5]([CH3:23])=[C:4]2[CH3:3])([CH3:20])[C:12]([CH3:19])=[C:13]([CH3:18])[C:14]=1[CH3:17]

Participants

5

Reactant 3

HCID 6417Pivalic acidHCID 8471TriethylamineHCID 178426003HCID 178426003, compound

Product 1

HCID 178447531HCID 178447531, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To a solution of bis(pentamethylcyclopentadienyl)zirconium dichloride (0.865 g, 2.001 mmol) and pivalic acid (0.685 g, 6.710 mmol) in toluene (30 ml) at 40° C. was added triethylamine (0.726 g, 7.174 mmol) with stirring. A white precipitate formed immediately which was removed by filtration. The title compound was isolated as an off-white powder in 90% by evaporating the solvent and excess pivalic acid under vacuum at 65° C. The title compound such prepared exhibited purity above 98% based on NMR results. 1H NMR (toluene d8) δ1.83 (s, 30H), 1.30 (s, 18H).

Workup

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

Sources & evidence

ORD record
ord-41d99eedadc0401e9177a69ca5efc7b5
Source dataset
uspto-grants-2007_05
Patent number
US07220804B1

Reaction notes

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