HCID 131723810, compound → HCID 131723812, compound

HRID 1862078Notes

Reaction equation

HRID 1862078 reaction equation
[Cl-:1].[Cl-].[Zr+2:3].[CH:4]1([C:9]([CH:19]2[CH:23]=[CH:22][CH:21]=[CH:20]2)([CH2:11][CH2:12][CH2:13][O:14][Si](C)(C)C)[CH3:10])[CH:8]=[CH:7][CH:6]=[CH:5]1>C1(C)C=CC=CC=1>[Cl-:1].[Cl-:1].[Zr+2:3].[CH:19]1([C:9]([CH:4]2[CH:5]=[CH:6][CH:7]=[CH:8]2)([CH2:11][CH2:12][CH2:13][OH:14])[CH3:10])[CH:20]=[CH:21][CH:22]=[CH:23]1

Participants

3

Reactant 1

HCID 131723810HCID 131723810, compound

Product 1

HCID 131723812HCID 131723812, compoundYield 18.8%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

XPO 2407 silica, provided by Grace, (7.2 g) was placed in a 250 ml dark-coloured Schlenk flask and washed with toluene (2×200 ml). Toluene (150 ml) and a solution of 2,2-bis(cyclopentadienyl)-5-trimethylsiloxypentane zirconium dichloride (2.0 g, 0.0045 mol) in toluene (50 ml) were added and the slurry was stirred for 90 h. After this time the mixture was filtered and the solvent removed under vacuum. Affording a yellow solid (0.16 g, 9.5% yield). 1H NMR (CDCl3): Λ6.70 (C5H4, d, 4H), 5.83 (C5H4, d, 4H), 3.85 (CH2, t, 2H), 2.32 (CH2H m, 2H), 1.88 (CH2, m, 2H), 1.80 (CH3, s, 3H, 1.45 (OH, s, 1H).

Workup

  1. customXPO 2407 silica, provided by Grace, (7.2 g)
  2. customwas placed in a 250 ml dark-coloured Schlenk flask
  3. washwashed with toluene (2×200 ml)
  4. filtrationAfter this time the mixture was filtered
  5. customthe solvent removed under vacuum

Sources & evidence

ORD record
ord-9656a9e73bad494db7a39d1423b057e2
Source dataset
uspto-grants-2003_03
Patent number
US06534665B1

Reaction notes

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