HCID 15300442, compound → HCID 178441216, compound

HRID 1581467Notes

Reaction equation

HRID 1581467 reaction equation
C[Si]([O:5][C:6]1[C:11]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:10][C:9]([C:16]([CH3:19])([CH3:18])[CH3:17])=[CH:8][C:7]=1[P:20]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)(C)C.[O:33]1[CH2:37][CH2:36][CH2:35][CH2:34]1.[Cl-:38].[Cl-].[Cl-].[Cl-].[Zr+4:42]>O1CCCC1>[Cl-:38].[Cl-:38].[C:21]1([P:20]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:7]2[CH:8]=[C:9]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:10]=[C:11]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:6]=2[O:5][Zr+2:42][O:33][C:37]2[C:36]([C:12]([CH3:13])([CH3:14])[CH3:15])=[CH:35][C:34]([C:16]([CH3:19])([CH3:18])[CH3:17])=[CH:28][C:27]=2[P:20]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:6]=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

Participants

4

Reactant 2

HCID 15300442HCID 15300442, compoundHCID 86586626zirconium tetrachloride THF

Product 1

HCID 178441216HCID 178441216, compoundYield 58.1%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Conditions

Temperature
-30 °C

Procedure

Next, 0.98 g (2.11 millimole) of this 4,6-di-tert-butyl-2-diphenylphosphinophenyl trimethylsilyl ether was dissolved in 15 ml of dehydrated tetrahydrofuran under nitrogen flow, and the solution was cooled down to −30° C. Then, a dehydrated tetrahydrofuran solution of 0.4 g (1.06 millimole) of a zirconium tetrachloride tetrahydrofuran adduct was added thereto step by step, and the solution was stirred at a room temperature for one hour. Further, the solution was refluxed for 3 days by heating. The solvent was distilled off under reduced pressure, and the residue was recrystallized from dichloromethane/hexane, whereby obtained was 0.29 g (yield: 29.0%) of bis (2-diphenylphosphino-4,6-di-tert-butylphenoxy) zirconium dichloride.

Workup

  1. temperatureFurther, the solution was refluxed for 3 days
  2. temperatureby heating
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe residue was recrystallized from dichloromethane/hexane, whereby
  5. customobtained

Sources & evidence

ORD record
ord-bda6fbdf72d740c1990619adfc8e3d43
Source dataset
uspto-grants-2004_05
Patent number
US06730626B2

Reaction notes

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