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HCID 178504313, compound → HCID 178520413, compound

HRID 1953206
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Reaction equation

HRID 1953206 reaction equation
[Cl-:1].[Cl-].[CH:3]1([Zr+2:8][C:9]2([CH2:14][CH2:15][O:16][Si](C)(C)C)[CH:13]=[CH:12][CH:11]=[CH:10]2)[CH:7]=[CH:6][CH:5]=[CH:4]1>C1(C)C=CC=CC=1>[Cl-:1].[Cl-:1].[CH:3]1([Zr+2:8][C:9]2([CH2:14][CH2:15][OH:16])[CH:10]=[CH:11][CH:12]=[CH:13]2)[CH:7]=[CH:6][CH:5]=[CH:4]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

HCID 178504313HCID 178504313, compound

Product 1

HCID 178520413HCID 178520413, compoundYield 30%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

2.16 g (5.69 mmol) of the organocomplex (cyclopentadienyl)(trimethylsiloxyethylcyclopentadienyl) zirconium dichloride was added to a suspension of 2.9 g of Silica XPO 2407 in 75 ml of dry toluene at room temperature; the suspension immediately acquired a greenish-yellow color. The sample was maintained under continuous stirring at room temperature for 48 hours. The yellow solution was separated from the solid by filtration. The solution was brought to dryness and, after washing with three fractions of 15 ml of hexane, a dusty white solid was obtained. (0.57 g Yield: 30%) 1H-NMR: (Cl3CD): 1.65 (m,1H), 2.95 (t,2H), 4.05 (m,2H), 6.32 (m,2H), 6.35 (m,2H), 6.5 (s,5H).

Workup

  1. temperatureThe sample was maintained
  2. customThe yellow solution was separated from the solid by filtration
  3. washafter washing with three fractions of 15 ml of hexane
  4. customa dusty white solid was obtained

Sources & evidence

ORD record
ord-4241ccab23ab417684444a42b9b8d999
Source dataset
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06114555

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes