Ethylamine → HCID 123728622, compound

HRID 2273151Notes

Reaction equation

HRID 2273151 reaction equation
[CH2:1]([NH2:3])[CH3:2].Cl[SiH:5]1[N:9]([C:10]([CH3:13])([CH3:12])[CH3:11])[CH:8]=[CH:7][N:6]1[C:14]([CH3:17])([CH3:16])[CH3:15]>CCCCCC>[C:14]([N:6]1[CH:7]=[CH:8][N:9]([C:10]([CH3:13])([CH3:12])[CH3:11])[SiH:5]1[NH:3][CH2:1][CH3:2])([CH3:17])([CH3:16])[CH3:15]

Participants

4

Reactant 2

HCID 6341EthylamineHCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

Product 1

HCID 123728622HCID 123728622, compoundYield 96%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent2×

Procedure

In an argon atmosphere, 3.40 g (75.5 mmol) of ethylamine was dissolved in 30 mL of hexane, and a solution obtained by dissolving 5.78 g (24.8 mmol) of Si(tBuNCHCHNtBu)(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: 86° C./4.1×102 Pa) to obtain 1,3-di-tert-butyl-2-ethylamino-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)NHEt) as a pale yellow liquid (yielded amount: 5.77 g, yield: 96%).

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: 86° C./4.1×102 Pa)
  8. customto obtain

Sources & evidence

ORD record
ord-4a0ad653b0b34a09a18d40320e601514
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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