Potassium cyanate → HCID 123671386, compound

HRID 2273164Notes

Reaction equation

HRID 2273164 reaction equation
Cl[SiH:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[CH:5]=[CH:4][N:3]1[C:11]([CH3:14])([CH3:13])[CH3:12].[O-:15][C:16]#[N:17].[K+]>O1CCCC1>[C:11]([N:3]1[CH:4]=[CH:5][N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[SiH:2]1[N:17]=[C:16]=[O:15])([CH3:14])([CH3:13])[CH3:12]

Participants

4

Reactant 2

HCID 11378442Potassium cyanateHCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

Product 1

HCID 123671386HCID 123671386, compoundYield 83%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

In an argon atmosphere, 8.33 g (35.8 mmol) of Si(tBuNCHCHNtBu)(H)Cl was dissolved in 30 mL of tetrahydrofuran and after adding 3.19 g (purity: 96%, 37.8 mmol) of potassium cyanate, the mixture was stirred for 15 hours under heating and refluxing. 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: 85° C./3.3×102 Pa) to obtain 1,3-di-tert-butyl-2-isocyanato-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)NCO) as a colorless liquid (yielded amount: 7.07 g, yield: 83%). The thus-obtained Si(tBuNCHCHNtBu)(H)NCO was measured for the 1H and 13C NMR spectra, as a result, these spectra agreed with spectra of that obtained in Example-29.

Workup

  1. temperatureunder heating
  2. temperaturerefluxing
  3. customInsoluble matters produced
  4. customwere separated by filtration
  5. customthe solvent was removed by distillation from the filtrate under atmospheric pressure
  6. distillationThe obtained residue was distilled under reduced pressure (distillation temperature: 85° C./3.3×102 Pa)
  7. customto obtain

Sources & evidence

ORD record
ord-d40778652e134e91923bcb5fa2194402
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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