Trichlorosilane → 1,3-Diaza-2-silacyclopent-4-ene, 2-chloro-1,3-bis(1-methylpropyl)-

In an argon atmosphere, a dilithium(N,N′-di-sec-butyl-1,2-vinylenediaminide) solution prepared according to the procedure and reagent quantities described in Reference Example-8 was added to a hexane (150 mL) solution containing 25.00 g (184.6 mmol) of trichlorosilane, and the mixture was stirred at room temperature for 6 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: 85° C./5×102 Pa) to obtain 2-chloro-1,3-di-sec-butyl-1,3-diaza-2-silacyclopent-4-ene (Si(sBuNCHCHNsBu)(H)Cl) as a pale yellow liquid (yielded amount: 18.10 g, yield: 42%). This product was a mixture of a plurality of isomers differing in the steric configuration from each other.

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: 85° C./5×102 Pa)
5. customto obtain

ORD record

ord-b3b25c3e1105424fbc8ba2638fb3fa48

Source dataset

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09120825B2