Tributyltin fluoride → HCID 178504582, compound

HRID 719083Notes

Reaction equation

HRID 719083 reaction equation
[Cl-].[Cl-].[CH3:3][SiH:4]([Zr+2:6]([CH:16]1[C:24]2[CH:19]([CH2:20][CH:21]=[CH:22][CH:23]=2)[CH2:18][CH2:17]1)[CH:7]1[C:15]2[CH:10]([CH2:11][CH:12]=[CH:13][CH:14]=2)[CH2:9][CH2:8]1)[CH3:5].C([Sn]([F:38])(CCCC)CCCC)CCC>ClCCl>[F-:38].[F-:38].[CH3:5][SiH:4]([Zr+2:6]([CH:7]1[C:15]2[CH:10]([CH2:11][CH:12]=[CH:13][CH:14]=2)[CH2:9][CH2:8]1)[CH:16]1[C:24]2[CH:19]([CH2:20][CH:21]=[CH:22][CH:23]=2)[CH2:18][CH2:17]1)[CH3:3]

Participants

4

Reactant 2

HCID 16120Tributyltin fluorideHCID 178504581HCID 178504581, compound

Product 1

HCID 178504582HCID 178504582, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a murky green-yellow solution of rac-dimethylsilyl-bis (tetrahydroindenyl) zirconium dichloride [DMS bis (THI) ZrCl2] (1.00 g, 2.19 mmol, 1.00 eq.) in dichloromethane (15 mL) was added tributyltin fluoride (1.42 g, 4.59 mmol, 2.10 eq.). The reaction lightened immediately. The reaction was stirred for one hour and was then filtered to give a straw-yellow solution and a small amount of brownish solid. The solution was then evaporated in vacuo, leaving a manila-colored, thick suspension. The suspension was washed with pentane (20 mL, then 3×5 mL) to give a white, micro crystalline solid. The solid was dried in vacuo to yield 0.76 g (82%). 1H NMR (CD2Cl2): δ 0.80 (s, 6H, SiMe2, 1.45–1.9 and 2.4–2.7 (br m, 16H, aliphatic-ring-H), 5.61 (d, 2H, cyclopentadienyl-ring-H), 6.27 (br s, 2H, cyclopentadienyl-ring-H). 19F NMR (CD2Cl2): δ 19.9 (s).

Workup

  1. filtrationwas then filtered
  2. customto give a straw-yellow solution
  3. customThe solution was then evaporated in vacuo
  4. customleaving a manila-colored, thick suspension
  5. washThe suspension was washed with pentane (20 mL
  6. custom3×5 mL) to give a white, micro crystalline solid
  7. customThe solid was dried in vacuo
  8. customto yield 0.76 g (82%)

Sources & evidence

ORD record
ord-948f7e175640492b98f7c9a38557aeb4
Source dataset
uspto-grants-2006_11
Patent number
US07132382B2

Reaction notes

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