Ammonia → HCID 123314264, compound

HRID 2273161Notes

Reaction equation

HRID 2273161 reaction equation
Cl[SiH:2]1[N:6]([C:7]([CH3:14])([CH3:13])[CH2:8][C:9]([CH3:12])([CH3:11])[CH3:10])[CH:5]=[CH:4][N:3]1[C:15]([CH3:22])([CH3:21])[CH2:16][C:17]([CH3:20])([CH3:19])[CH3:18].[NH3:23]>CCCCCC>[NH2:23][SiH:2]1[N:6]([C:7]([CH3:14])([CH3:13])[CH2:8][C:9]([CH3:12])([CH3:11])[CH3:10])[CH:5]=[CH:4][N:3]1[C:15]([CH3:22])([CH3:21])[CH2:16][C:17]([CH3:20])([CH3:19])[CH3:18]

Participants

4

Reactant 2

HCID 222Ammonia2×HCID 123708636HCID 123708636, compound

Product 1

HCID 123314264HCID 123314264, compoundYield 88%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

In an argon atmosphere, 5.42 g (15.7 mmol) of Si(tOctNCHCHNtOct)(H)Cl was dissolved in 20 mL of hexane. The resulting solution was deaerated by Freeze-Pump-Thaw cycling and after creating an ammonia atmosphere in the reaction vessel by connecting thereto a balloon having an internal volume of 5 L and being filled with ammonia, the solution was stirred at room temperature for 41 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: 115° C./1.2×102 Pa) to obtain 2-amino-1,3-bis(1,1,3,3-tetramethylbutyl)-1,3-diaza-2-silacyclopent-4-ene (Si(tOctNCHCHNtOct)(H)NH2) as a pale yellow liquid (yielded amount: 4.52 g, yield: 88%). The thus-obtained Si(tOctNCHCHNtOct)(H)NH2 was measured for the 1H and 13C NMR spectra, as a result, these spectra agreed with spectra of that obtained in Example-24.

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: 115° C./1.2×102 Pa)
  5. customto obtain

Sources & evidence

ORD record
ord-627441564cb44f41a6d9758f70532d51
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

Loading…