Hexane → HCID 102348198, compound

HRID 2273149Notes

Reaction equation

HRID 2273149 reaction equation
[NH2-:1].[Li+].Cl[SiH:4]1[N:8]([C:9]([CH3:12])([CH3:11])[CH3:10])[CH:7]=[CH:6][N:5]1[C:13]([CH3:16])([CH3:15])[CH3:14].CCCCCC>COCCOC>[NH2:1][SiH:4]1[N:8]([C:9]([CH3:12])([CH3:11])[CH3:10])[CH:7]=[CH:6][N:5]1[C:13]([CH3:16])([CH3:15])[CH3:14]

Participants

5

Reactant 3

HCID 8058HexaneHCID 24532Lithium amideHCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

Product 1

HCID 102348198HCID 102348198, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 80711,2-DimethoxyethaneSolvent

Procedure

In an argon atmosphere, 505 mg (purity: 95%, 20.9 mmol) of lithium amide was suspended in 20 mL of 1,2-dimethoxyethane and after adding 4.65 g (20.0 mmol) of Si(tBuNCHCHNtBu)(H)Cl, the mixture was stirred at room temperature for 2 hours. Subsequently, 20 mL of hexane was added to the reaction mixture, and the mixture was stirred at room temperature for 10 minutes. 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: 78° C./3.8×102 Pa) to obtain 2-amino-1,3-di-tert-butyl-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)NH2) as a pale yellow liquid (yielded amount: 3.93 g, yield: 92%).

Workup

  1. stirringthe mixture was stirred at room temperature for 10 minutes
  2. customInsoluble matters produced
  3. customwere separated by filtration
  4. customthe solvent was removed by distillation from the filtrate under atmospheric pressure
  5. distillationThe obtained residue was distilled under reduced pressure (distillation temperature: 78° C./3.8×102 Pa)
  6. customto obtain

Sources & evidence

ORD record
ord-48348288e6ca4a47aa1219a2c25955cc
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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