Sodium thiocyanate → HCID 123311522, compound

HRID 2273166Notes

Reaction equation

HRID 2273166 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].[S-: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]=[S:15])([CH3:14])([CH3:13])[CH3:12]

Participants

4

Reactant 2

HCID 516871Sodium thiocyanateHCID 713346111,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole

Product 1

HCID 123311522HCID 123311522, compoundYield 90%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

In an argon atmosphere, 6.10 g (26.2 mmol) of Si(tBuNCHCHNtBu)(H)Cl was dissolved in 20 mL of tetrahydrofuran and after adding 2.15 g (purity: 99%, 26.3 mmol) of sodium thiocyanate, the mixture was stirred at room temperature for 14 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: 108° C./3.3×102 Pa) to obtain 1,3-di-tert-butyl-2-thioisocyanato-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)NCS) as a pale yellow liquid (yielded amount: 6.05 g, yield: 90%).

Workup

  1. customInsoluble matters produced
  2. customwere separated by filtration
  3. customthe solvent was removed by distillation from the filtrate under atmospheric pressure
  4. distillationThe obtained residue was distilled under reduced pressure (distillation temperature: 108° C./3.3×102 Pa)
  5. customto obtain

Sources & evidence

ORD record
ord-3658c3b83284496cb6a7b3401dd642d4
Source dataset
uspto-grants-2015_09
Patent number
US09120825B2

Reaction notes

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