Titanium Tetrachloride → HCID 18175992, compound

HRID 1033867Notes

Reaction equation

HRID 1033867 reaction equation
[Ti:1](Cl)(Cl)(Cl)Cl.[CH2:6]([N-:9][CH2:10][CH2:11][CH3:12])[CH2:7][CH3:8].[Li+]>C1(C)C=CC=CC=1>[CH2:6]([N-:9][CH2:10][CH2:11][CH3:12])[CH2:7][CH3:8].[CH2:6]([N-:9][CH2:10][CH2:11][CH3:12])[CH2:7][CH3:8].[CH2:6]([N-:9][CH2:10][CH2:11][CH3:12])[CH2:7][CH3:8].[CH2:6]([N-:9][CH2:10][CH2:11][CH3:12])[CH2:7][CH3:8].[Ti+4:1]

Participants

4

Reactant 2

HCID 24193Titanium TetrachlorideHCID 10898668HCID 10898668, compound

Product 1

HCID 18175992HCID 18175992, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

The same apparatus described in Step (1) of Example C is used in this procedure. The 250 mL dropping funnel is charged with toluene, 100 mL, and titanium tetrachloride, 10.7 g (0.0562 mole). This is added dropwise to the flask containing lithium di-n-propylamide while stirring magnetically. Total additions times are typically 30 minutes. The mixture is refluxed for 1.5 hours. All volatiles are removed by distillation and under vacuum to give a deeply colored brown, oily residue. The residue is extracted with hexane, 2×150 mL, then filtered from the lithium salts. The extracts are combined and solvent is removed under vacuum. The remaining oil is transferred to a small scale distillation apparatus. Vacuum distillation at 157° C. and 0.05 mm Hg gave the product as an orange-brown liquid, titanium tetrakis(dipropylamide).

Workup

  1. additionThis is added dropwise to the flask
  2. temperatureThe mixture is refluxed for 1.5 hours
  3. customAll volatiles are removed by distillation and under vacuum
  4. customto give a deeply colored brown, oily residue
  5. extractionThe residue is extracted with hexane, 2×150 mL
  6. filtrationfiltered from the lithium salts
  7. customsolvent is removed under vacuum
  8. distillationThe remaining oil is transferred to a small scale distillation apparatus
  9. distillationVacuum distillation at 157° C.

Sources & evidence

ORD record
ord-821e1af1e96a41508d0e2f4a4a154475
Source dataset
uspto-grants-1994_05
Patent number
US05312938

Reaction notes

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