HCID 178418361, compound → HCID 178421916, compound

HRID 54609Notes

Reaction equation

HRID 54609 reaction equation
[Cl-:1].[Cl-].[CH3:3][Zr:4]([CH3:26])(=[SiH2:25])([CH:15]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[C:16]1[CH3:24])[CH:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[C:6]1[CH3:14].[H][H]>ClCCl.[Pt]=O>[Cl-:1].[Cl-:1].[CH3:26][Zr:4]([CH3:3])(=[SiH2:25])([CH:5]1[C:13]2[CH:8]([CH2:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][CH:6]1[CH3:14])[CH:15]1[C:23]2[CH:18]([CH2:19][CH:20]=[CH:21][CH:22]=2)[CH2:17][CH:16]1[CH3:24]

Participants

5

Reactant 2

HCID 178418361HCID 178418361, compoundHCID 178421920HCID 178421920, compound

Product 1

HCID 178421916HCID 178421916, compound

Reagents, catalysts & solvents 2

HCID 82844Platinum oxide (PtO)CatalystHCID 6344DichloromethaneSolvent

Procedure

A 0.5 g portion of dimethylsilylenebis(2-methylindenyl)zirconium dichloride obtained in Example 1 was dissolved in 250 ml of dichloromethane and introduced into a 1.0 liter autoclave, and 0.5 g of platinum oxide was then introduced. Hydrogen pressure was increased to 50 kg/cm2 ·G to carry out hydrogenation at 30° C. for 4 hours. After the reaction was completed, the slurry was filtered to separate the platinum catalyst, and the solvent was removed by distillation. The product was dissolved in 200 ml of toluene, and the solution was concentrated into about 50 ml, which was left standing overnight at -20° C. to form crystals. The crystals formed were filtered, and desiccated to give 0.22 g of the title product.

Workup

  1. additionwas then introduced
  2. customat 30° C.
  3. customfor 4 hours
  4. filtrationthe slurry was filtered
  5. customto separate the platinum catalyst
  6. customthe solvent was removed by distillation
  7. dissolutionThe product was dissolved in 200 ml of toluene
  8. concentrationthe solution was concentrated into about 50 ml, which
  9. waitwas left
  10. customto form crystals
  11. customThe crystals formed
  12. filtrationwere filtered

Sources & evidence

ORD record
ord-8578861185304ca994f06c097a64bb65
Source dataset
uspto-grants-1997_04
Patent number
US05623022

Reaction notes

Loading…