Methylgallium dichloride → Bis-(3-dimethylaminopropyl)methylgallium

HRID 1458510Notes

Reaction equation

HRID 1458510 reaction equation
[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][CH2:5][Li].[Cl-].[Cl-].[CH3:10][Ga+2:11]>CCCCC.C1C=CC=CC=1>[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][CH2:5][Ga:11]([CH2:5][CH2:4][CH2:3][N:2]([CH3:7])[CH3:1])[CH3:10]

Participants

5

Reactant 2

HCID 178477772Methylgallium dichlorideHCID 178506872HCID 178506872, compound

Product 1

HCID 14531890Bis-(3-dimethylaminopropyl)methylgallium

Reagents, catalysts & solvents 2

HCID 241BenzeneSolventHCID 8003PentaneSolvent

Procedure

5 g of 3-dimethylaminopropyllithium (53.7 mmol) are suspended in 40 ml of pentane, and a solution of 4 g of methylgallium dichloride (25.7 mmol) in 20 ml of benzene is added dropwise. The mixture is first stirred at room temperature for one hour and then boiled under reflux for 6 hours. After cooling, the lithium chloride and excess lithium salt are filtered off and the solvent is stripped off in vacuo. The residue which remains is sublimed in vacuo at an oil bath temperature of 60° C. Bis-(3-dimethylaminopropyl)methylgallium is obtained as a white solid of melting point 52° C.

Workup

  1. temperatureunder reflux for 6 hours
  2. temperatureAfter cooling
  3. filtrationthe lithium chloride and excess lithium salt are filtered off
  4. customThe residue which remains is sublimed in vacuo at an oil bath
  5. customtemperature of 60° C

Sources & evidence

ORD record
ord-650a2a53f26c4523806b27c73bbb10e0
Source dataset
uspto-grants-1998_12
Patent number
US05851946

Reaction notes

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