Ethylamine → HCID 123737078, compound

HRID 2273162Notes

Reaction equation

HRID 2273162 reaction equation
[CH2:1]([NH2:3])[CH3:2].Cl[SiH:5]1[N:9]([C:10]([CH3:17])([CH3:16])[CH2:11][C:12]([CH3:15])([CH3:14])[CH3:13])[CH:8]=[CH:7][N:6]1[C:18]([CH3:25])([CH3:24])[CH2:19][C:20]([CH3:23])([CH3:22])[CH3:21]>CCCCCC>[CH3:24][C:18]([N:6]1[CH:7]=[CH:8][N:9]([C:10]([CH3:17])([CH3:16])[CH2:11][C:12]([CH3:15])([CH3:14])[CH3:13])[SiH:5]1[NH:3][CH2:1][CH3:2])([CH3:25])[CH2:19][C:20]([CH3:23])([CH3:22])[CH3:21]

Participants

4

Reactant 2

HCID 6341EthylamineHCID 123708636HCID 123708636, compound

Product 1

HCID 123737078HCID 123737078, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent2×

Procedure

In an argon atmosphere, 6.80 g (151 mmol) of ethylamine was dissolved in 20 mL of hexane, and a solution obtained by dissolving 5.26 g (15.2 mmol) of Si(tOctNCHCHNtOct)(H)Cl in 10 mL of hexane was added thereto at −20° C. After stirring at room temperature for 12 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: 128° C./1.4×102 Pa) to obtain 1,3-bis(1,1,3,3-tetramethylbutyl)-2-ethylamino-1,3-diaza-2-silacyclopent-4-ene (Si(tOctNCHCHNtOct)(H)NHEt) as a pale yellow liquid (yielded amount: 5.22 g, yield: 97%).

Workup

  1. customa solution obtained
  2. additionwas added
  3. customat −20° C
  4. custominsoluble matters produced
  5. customwere separated by filtration
  6. customthe solvent was removed by distillation from the filtrate under atmospheric pressure
  7. distillationThe obtained residue was distilled under reduced pressure (distillation temperature: 128° C./1.4×102 Pa)
  8. customto obtain

Sources & evidence

ORD record
ord-23e2d29104084545b7e807c13bdaa719
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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