1270-98-0 → HCID 178455543, compound

HRID 325056Notes

Reaction equation

HRID 325056 reaction equation
[O:1]([Si:3]([C:12]([CH3:15])([CH3:14])[CH3:13])([C:8]([CH3:11])([CH3:10])[CH3:9])[C:4]([CH3:7])([CH3:6])[CH3:5])[Na].[CH-:16]1[CH:20]=[CH:19][CH:18]=[CH:17]1.[Cl:21][Ti+:22](Cl)Cl>C1(C)C=CC=CC=1>[Cl-:21].[Cl-:21].[CH:16]1([Ti+2:22][O:1][Si:3]([C:12]([CH3:15])([CH3:14])[CH3:13])([C:8]([CH3:11])([CH3:10])[CH3:9])[C:4]([CH3:7])([CH3:6])[CH3:5])[CH:20]=[CH:19][CH:18]=[CH:17]1

Participants

4

Reactant 2

HCID 791521270-98-0HCID 178455542HCID 178455542, compound

Product 1

HCID 178455543HCID 178455543, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Conditions

Temperature
23 °C

Procedure

NaOSitBu3 (0.502 g, 2.106 mmol, prepared by reacting Na and tBu3SiOH in refluxing hexane) in toluene (20 mL) was added to a toluene solution (20 mL) of CpTiCl3 (0.462 g, 2.106 mmol) at −78° C. The solution was warmed to 23° C. and stirred for about 5 hours. The solution was pumped to dryness and the residue was extracted with hexane. The hexane solution was concentrated to ˜2 mL and the product crystallized as yellow-orange crystals at −70° C. Yield was 0.79g, 94%. 1H NMR (C7D8, δ): 6.22 (s, 5H), 1.17 (s, 27H).

Workup

  1. extractionthe residue was extracted with hexane
  2. concentrationThe hexane solution was concentrated to ˜2 mL
  3. customthe product crystallized as yellow-orange crystals at −70° C

Sources & evidence

ORD record
ord-04a07e09512c4368adfab6059536ee0a
Source dataset
uspto-grants-2001_04
Patent number
US06221985B1

Reaction notes

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