Sodium Cyanate → HCID 123671386, compound

HRID 2273163Notes

Reaction equation

HRID 2273163 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].[Na+]>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 517096Sodium CyanateHCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

Product 1

HCID 123671386HCID 123671386, compoundYield 90%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

In an argon atmosphere, 7.69 g (33.0 mmol) of Si(tBuNCHCHNtBu)(H)Cl was dissolved in 30 mL of tetrahydrofuran and after adding 2.58 g (purity: 90%, 35.7 mmol) of sodium cyanate, the mixture was stirred for 8 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: 7.09 g, yield: 90%).

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-960e214073ea4a35a7a7a1f09be0a0b6
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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