1,2-Dimethoxyethane → HCID 178504313, compound

HRID 1348537Notes

Reaction equation

HRID 1348537 reaction equation
[Cl-:1].[Cl-].[Cl-].[CH:4]1([Zr+3:9])[CH:8]=[CH:7][CH:6]=[CH:5]1.C(COC)OC.[CH3:16][Si:17]([CH3:27])([CH3:26])[O:18][CH2:19][CH2:20][C-:21]1[CH:25]=[CH:24][CH:23]=[CH:22]1.[K+]>C1(C)C=CC=CC=1>[Cl-:1].[Cl-:1].[CH:4]1([Zr+2:9][C:21]2([CH2:20][CH2:19][O:18][Si:17]([CH3:16])([CH3:27])[CH3:26])[CH:22]=[CH:23][CH:24]=[CH:25]2)[CH:8]=[CH:7][CH:6]=[CH:5]1

Participants

5

Reactant 3

HCID 80711,2-DimethoxyethaneHCID 86199137Potassium (2-trimethylsiloxy-ethyl)-cyclopentadienideHCID 178478629HCID 178478629, compound

Product 1

HCID 178504313HCID 178504313, compoundYield 27%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

To a suspension of 3.52 g (10 mmol) of an adduct of cyclopentadienyl zirconium trichloride with dimethoxyethane in toluene, a suspension of 2.2 g (10 mmol) of potassium (2-trimethylsiloxy-ethyl)-cyclopentadienide in toluene is added. The addition is carried out at −78° C. An orange-brown suspension is immediately formed; it is maintained under stirring for 12 hours; then it is left settling and it is filtered. The obtained orange solution is concentrated up to 5 ml and hexane is added, so that a brown solid is obtained. (1.1 g, 2.7 mmol. Yield: 27%). 1H-NMR: 6.00 (t, 2H), 5.87 (s, 5H), 5.67 (t, 2H), 3.66 (t, 2H), 2.92 (t, 2H), 0.11 (s, 9H). Mass spectrum. M+-65: (343): 33%.

Workup

  1. additionis added
  2. additionThe addition
  3. customis carried out at −78° C
  4. customAn orange-brown suspension is immediately formed
  5. temperatureit is maintained
  6. waitthen it is left
  7. filtrationit is filtered
  8. concentrationThe obtained orange solution is concentrated up to 5 ml and hexane
  9. additionis added, so that a brown solid
  10. customis obtained

Sources & evidence

ORD record
ord-1300e5691eec40cbacbf276870028817
Source dataset
uspto-grants-2007_05
Patent number
US07211538B2

Reaction notes

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