Hexane → HCID 178478628, compound

HRID 1354512Notes

Reaction equation

HRID 1354512 reaction equation
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[CH2:7]([Sn]([Cl:20])(CCCC)CCCC)[CH2:8][CH2:9]C.[Cl-:21].[Cl-].[Cl-].[Cl-].[Zr+4:25]>C(Cl)Cl>[Cl-:20].[Cl-:21].[Cl-:20].[CH:3]1([Zr+3:25])[C:2]2[C:6](=[CH:7][CH:8]=[CH:9][CH:1]=2)[CH:5]=[CH:4]1

Participants

5

Reactant 3

HCID 8058HexaneHCID 15096Tributyltin ChlorideHCID 9856075Zirconium chloride (ZrCl4), (T-4)-

Product 1

HCID 178478628HCID 178478628, compoundYield 88%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

After adding litiumidenide (IndLi) powder (17.52 g, 0.144 mol) and hexane (300 ml) into a 500 mL flask under nitrogen atmosphere, tributyltin chloride (41 ml, 0.145 mol) was injected into the above mentioned flask with syringe slowly. The mixture is stirred at room temperature for 48 hours. Yellowish oil type product was obtained by a series of processes, such as separating the organic liquid by filtering reaction mixture and removing volatile from filtrate. Then the obtained yellowish oil type product was diluted with methylenedichloride (200 ml), and zirconium tetrachloride (ZrCl4, 33.03 g, 0.142 mol) was added. The mixture is stirred at room temperature for 48 hours. Indenylzirconium trichloride (IndZrCl3, 39.5 g, yield: 88%) was obtained by a series of processes, such as removing the volatile from reaction mixture, slurrifying by adding hexane (200 ml), filtering, collecting scarlet colored solid powder and drying.

Workup

  1. customYellowish oil type product was obtained by a series of processes
  2. customsuch as separating the organic liquid
  3. filtrationby filtering
  4. customreaction mixture
  5. customremoving volatile from filtrate
  6. additionwas added
  7. stirringThe mixture is stirred at room temperature for 48 hours

Sources & evidence

ORD record
ord-337927da00dd48c2867b2dbd4057b557
Source dataset
uspto-grants-2007_05
Patent number
US07223824B2

Reaction notes

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