Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trichlorosilane | HCID 24811 | — |
| Reactant | Sodium Cyanate | HCID 517096 | — |
| Reactant | Lithium | HCID 3028194 | — |
| Reactant | HCID 72325861 | HCID 72325861 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 123671386 | HCID 123671386 | 80% |
Reaction Steps
In an argon atmosphere, a dilithium(N,N′-di-tert-butyl-1,2-vinylenediaminide) solution prepared by using 32.16 g of tBuNCHCHNtBu, 250 mL of tetrahydrofuran and 2.67 g of lithium according to the procedure described in Reference Example-9 was added to a hexane (30 mL) solution containing 25.12 g (185.5 mmol) of trichlorosilane, and the mixture was stirred at room temperature for 3 hours. To this reaction mixture, 14.47 g (purity: 96%, 213.7 mmol) of sodium cyanate was added, and the mixture was stirred for 4 hours under heating an 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: 35.44 g, yield: 80%). 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 those obtained in Example-29 and Example-30.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09120825B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-8b92821f12ca42f1bb0ee1c9c94efe99 |
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| Source note | uspto-grants-2015_09 |
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