Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | Trichlorosilane | HCID 24811 | — |
| Reactant | Lithium | HCID 3028194 | — |
| Reactant | HCID 72325861 | HCID 72325861 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 123172080 | HCID 123172080 | 60% |
Reaction Steps
In an argon atmosphere, a dilithium(N,N′-di-tert-butyl-1,2-vinylenediaminide) solution prepared by using 32.00 g of tBuNCHCHNtBu, 50 mL of tetrahydrofuran, 150 mL of hexane and 2.67 g of lithium according to the procedure described in Reference Example-9 was added to a hexane (120 mL) solution containing 25.20 g (186.0 mmol) of trichlorosilane, and the mixture was stirred at room temperature for 4 hours. To this reaction mixture, 30.00 g (410.2 mmol) of diethylamine was added, and the mixture was stirred at room temperature for 5 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: 102° C./4.0×102 Pa) to obtain 1,3-di-tert-butyl-2-diethylamino-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)NEt2) as a pale yellow liquid (yielded amount: 30.29 g, yield: 60%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09120825B2 |
|---|
| Source dataset | uspto-grants-2015_09 |
|---|
| ORD ID | ord-75eac1664d8c4cf780aa8616ffe51e93 |
|---|
| Source note | uspto-grants-2015_09 |
|---|