Hexane → HCID 123314264, compound

HRID 2273160Notes

Reaction equation

HRID 2273160 reaction equation
[NH2-:1].[Li+].Cl[SiH:4]1[N:8]([C:9]([CH3:16])([CH3:15])[CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH:7]=[CH:6][N:5]1[C:17]([CH3:24])([CH3:23])[CH2:18][C:19]([CH3:22])([CH3:21])[CH3:20].CCCCCC>COCCOC>[NH2:1][SiH:4]1[N:8]([C:9]([CH3:16])([CH3:15])[CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH:7]=[CH:6][N:5]1[C:17]([CH3:24])([CH3:23])[CH2:18][C:19]([CH3:22])([CH3:21])[CH3:20]

Participants

5

Reactant 3

HCID 8058HexaneHCID 24532Lithium amideHCID 123708636HCID 123708636, compound

Product 1

HCID 123314264HCID 123314264, compoundYield 87%

Reagents, catalysts & solvents 1

HCID 80711,2-DimethoxyethaneSolvent

Procedure

In an argon atmosphere, 439 mg (purity: 95%, 18.2 mmol) of lithium amide was suspended in 20 mL of 1,2-dimethoxyethane and after adding 6.07 g (17.6 mmol) of Si(tOctNCHCHNtOct)(H)Cl, the mixture was stirred at room temperature for 4 hours. To the reaction mixture, 20 mL of hexane was added, 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: 116° C./1.3×102 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: 4.99 g, yield: 87%).

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: 116° C./1.3×102 Pa)
  6. customto obtain

Sources & evidence

ORD record
ord-8711d127b8b144049362f0f047648e39
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

Loading…