Trichlorosilane → 1,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

HRID 2273144Notes

Reaction equation

HRID 2273144 reaction equation
[C:1]([N-:5][CH:6]=[CH:7][N-:8][C:9]([CH3:12])([CH3:11])[CH3:10])([CH3:4])([CH3:3])[CH3:2].[Li+].[Li+].[Cl:15][SiH:16](Cl)Cl>CCCCCC>[Cl:15][SiH:16]1[N:5]([C:1]([CH3:3])([CH3:4])[CH3:2])[CH:6]=[CH:7][N:8]1[C:9]([CH3:12])([CH3:11])[CH3:10]

Participants

4

Reactant 2

HCID 24811TrichlorosilaneHCID 72325861HCID 72325861, compound

Product 1

HCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasiloleYield 83%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

In an argon atmosphere, a dilithium(N,N′-di-tert-butyl-1,2-vinylenediaminide) solution prepared according to the procedure and reagent quantities described in Reference Example-9 was added to a hexane (50 mL) solution containing 25.20 g (186.0 mmol) of trichlorosilane, and the mixture was stirred at room temperature for 3 hours. Insoluble matters produced were separated by filtration, and the solvent was removed by distillation from the filtrate under atmospheric pressure. The obtained residue was distilled under reduced pressure (distillation temperature: 80° C./3.8×102 Pa) to obtain 2-chloro-1,3-di-tert-butyl-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)Cl) as a colorless liquid (yielded amount: 35.58 g, yield: 83%).

Workup

  1. customInsoluble matters produced
  2. customwere separated by filtration
  3. customthe solvent was removed by distillation from the filtrate under atmospheric pressure
  4. distillationThe obtained residue was distilled under reduced pressure (distillation temperature: 80° C./3.8×102 Pa)
  5. customto obtain

Sources & evidence

ORD record
ord-73ccfe17e6f848d889aaa3431f0a3edb
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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