Dimethylamine → HCID 123537448, compound

HRID 2273168Notes

Reaction equation

HRID 2273168 reaction equation
Cl[SiH:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[CH:5]=[CH:4][N:3]1[C:11]([CH3:14])([CH3:13])[CH3:12].[CH3:15][NH:16][CH3:17]>CCCCCC>[C:11]([N:3]1[CH:4]=[CH:5][N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[SiH:2]1[N:16]([CH3:17])[CH3:15])([CH3:14])([CH3:13])[CH3:12]

Participants

4

Reactant 2

HCID 674Dimethylamine2×HCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

Product 1

HCID 123537448HCID 123537448, compoundYield 91%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

In an argon atmosphere, 3.98 g (17.1 mmol) of Si(tBuNCHCHNtBu)(H)Cl was dissolved in 20 mL of hexane. The resulting solution was deaerated by Freeze-Pump-Thaw cycling and after creating a dimethylamine atmosphere in the reaction vessel by connecting thereto a balloon having an internal volume of 5 L and being filled with dimethylamine, the solution was stirred at room temperature for 20 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: 84° C./4.7×102 Pa) to obtain 1,3-di-tert-butyl-2-dimethylamino-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)NMe2) as a colorless liquid (yielded amount: 3.76 g, yield: 91%).

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: 84° C./4.7×102 Pa)
  5. customto obtain

Sources & evidence

ORD record
ord-874a722e269a41b0a8166bc845abf63f
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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