HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole → 1,3-Di-tert-butyl-2-(prop-1-en-2-yl)-1,3-diaza-2-silacyclopent-4-ene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,3-Di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazasilole | HCID 71334611 | — |
| Reactant | HCID 178420658 | HCID 178420658 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | 1,3-Di-tert-butyl-2-(prop-1-en-2-yl)-1,3-diaza-2-silacyclopent-4-ene | HCID 123717700 | 47% |
Reaction Steps
In an argon atmosphere, 8.71 g (37.4 mmol) of Si(tBuNCHCHNtBu)(H)Cl was dissolved in 20 mL of hexane and after adding a (prop-1-en-2-yl)magnesium bromide tetrahydrofuran solution (0.57 mol/L, 69.0 mL, 39.3 mmol), the resulting solution was refluxed 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: 80° C./4.3×102 Pa) to obtain 1,3-di-tert-butyl-2-(prop-1-en-2-yl)-1,3-diaza-2-silacyclopent-4-ene (Si(tBuNCHCHNtBu)(H)C(CH3)CH2) as a yellow liquid (yielded amount: 4.18 g, yield: 47%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09120825B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-ec5e4838d70f430f913a09a8d90a057e |
| Source note | uspto-grants-2015_09 |