Ethylamine → HCID 123204542, compound

HRID 2273159Notes

Reaction equation

HRID 2273159 reaction equation
[CH2:1]([NH2:3])[CH3:2].Cl[SiH:5]1[N:9]([CH:10]([CH2:12][CH3:13])[CH3:11])[CH:8]=[CH:7][N:6]1[CH:14]([CH2:16][CH3:17])[CH3:15]>CCCCCC>[CH:14]([N:6]1[CH:7]=[CH:8][N:9]([CH:10]([CH2:12][CH3:13])[CH3:11])[SiH:5]1[NH:3][CH2:1][CH3:2])([CH2:16][CH3:17])[CH3:15]

Participants

4

Reactant 2

HCID 6341EthylamineHCID 1232513791,3-Diaza-2-silacyclopent-4-ene, 2-chloro-1,3-bis(1-methylpropyl)-

Product 1

HCID 123204542HCID 123204542, compoundYield 87%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent2×

Procedure

In an argon atmosphere, 3.30 g (73.2 mmol) of ethylamine was dissolved in 30 mL of hexane, and a solution obtained by dissolving 6.21 g (26.7 mmol) of Si(sBuNCHCHNsBu)(H)Cl in 5 mL of hexane was added thereto at −20° C. After stirring at room temperature for 2 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: 92-96° C./4.0×102 Pa) to obtain 1,3-di-sec-butyl-2-ethylamino-1,3-diaza-2-silacyclopent-4-ene (Si(sBuNCHCHNsBu)(H)NHEt) as a pale yellow liquid (yielded amount: 5.61 g, yield: 87%). This product was a mixture of a plurality of isomers differing in the steric configuration from each other.

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: 92-96° C./4.0×102 Pa)
  8. customto obtain

Sources & evidence

ORD record
ord-e55529ecba484142a245d7890b3a30be
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

Loading…