Chlorotrimethylsilane → HCID 178504324, compound

HRID 1879581Notes

Reaction equation

HRID 1879581 reaction equation
[Sb:1].[H-].[Li+].[CH3:4][Si:5]([CH3:8])([CH3:7])Cl>O1CCCC1>[CH3:4][Si:5]([Sb:1]([Si:5]([CH3:8])([CH3:7])[CH3:4])[Si:5]([CH3:8])([CH3:7])[CH3:4])([CH3:8])[CH3:7]

Participants

5

Reactant 3

HCID 6397ChlorotrimethylsilaneHCID 62714Lithium hydrideHCID 5354495Antimony2×

Product 1

HCID 178504324HCID 178504324, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
-20 °C

Procedure

1.22 g (0.01 mol) of 200 mesh antimony powder, 0.72 g (0.03 mol) of lithium hydride, and 40 ml of tetrahydrofuran (THF) were placed in a 100 ml flask. With stirring, the mixture was refluxed for 4 hours. All of the black powder constituting antimony disappeared, and a muddy colored precipitate was formed. Then, the mixture was cooled down to −20° C.; 3.3 g (0.03 mol) of trimethylchlorosilane was added. The mixture was allowed to warm up to room temperature. After stirring for 4 hours, the mixture was filtered under inert atmosphere. The solvent was removed by distillation. Tris(trimethylsilyl)antimony was purified by vacuum distillation.

Workup

  1. temperaturethe mixture was refluxed for 4 hours
  2. customa muddy colored precipitate was formed
  3. temperatureto warm up to room temperature
  4. stirringAfter stirring for 4 hours
  5. filtrationthe mixture was filtered under inert atmosphere
  6. customThe solvent was removed by distillation
  7. distillationTris(trimethylsilyl)antimony was purified by vacuum distillation

Sources & evidence

ORD record
ord-7ba8daf86dcc416f89e88c668cdbe9f7
Source dataset
uspto-grants-2012_11
Patent number
US08318252B2

Reaction notes

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