Titanium Tetrachloride → Chlorotitanium(3+);tris(diethylazanide)

HRID 1033870Notes

Reaction equation

HRID 1033870 reaction equation
[CH2:1]([N-:3][CH2:4][CH3:5])[CH3:2].[CH2:6]([N-:8][CH2:9][CH3:10])[CH3:7].[CH2:11]([N-:13][CH2:14][CH3:15])[CH3:12].C([N-]CC)C.[Ti+4].[Ti:22](Cl)(Cl)(Cl)[Cl:23]>C1(C)C=CC=CC=1>[CH2:1]([N-:3][CH2:4][CH3:5])[CH3:2].[CH2:6]([N-:8][CH2:9][CH3:10])[CH3:7].[CH2:11]([N-:13][CH2:14][CH3:15])[CH3:12].[Cl:23][Ti+3:22]

Participants

4

Reactant 2

HCID 24193Titanium TetrachlorideHCID 123216ethanamine, n-ethyl-, titanium(4+) salt

Product 1

HCID 11781534Chlorotitanium(3+);tris(diethylazanide)

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

A 250 mL Schlenk flask is charged with toluene, 100 mL, and titanium tetrakis(diethylamide), 6.21 g (18.5 mmole). To the magnetically stirred solution is added titanium tetrachloride, 1.17 g (6.15 mmole) resulting in a gradual darkening of the solution. The mixture is stirred 1 hour while refluxing. All volatiles are removed under vacuum at room temperature leaving a yellow-brown oil. The oil is transferred to a micro distillation apparatus and distilled under vacuum. A yellow-brown liquid is obtained which distills at 112° to 118° C. (at 0.025 mm Hg). The product is determined to be chloro titanium tris(diethylamide).

Workup

  1. customresulting in a gradual darkening of the solution
  2. temperaturewhile refluxing
  3. customAll volatiles are removed under vacuum at room temperature
  4. customleaving a yellow-brown oil
  5. distillationdistilled under vacuum
  6. customA yellow-brown liquid is obtained which
  7. distillationdistills at 112° to 118° C. (at 0.025 mm Hg)

Sources & evidence

ORD record
ord-b0bb05784de94e8e932f8ba1218e589e
Source dataset
uspto-grants-1994_05
Patent number
US05312938

Reaction notes

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