Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fluorene | HCID 6853 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Dimethyl Ether | HCID 8254 | — |
| Product | HCID 178506660 | HCID 178506660 | — |
Reaction Steps
Here 5 g (30 mmol) fluorene, dissolved in dimethyl ether, was reacted for three hours with 18.8 ml of butyllithium (1.6M in hexane). The solvent was evaporated to yield yellow fluorenyl lithium. Then 11.4 g (45 mmol) of Ph2SiCl2, i.e. diphenyl dichloro silane, was dissolved in 200 ml of pentane and the solid fluorenyl lithium was added in one portion to the pentane solution. After stirring for one hour, the mixture was filtered, the precipitated LiCl was eluted with 50 ml of ether, and the solvent evaporated from the combined organic layers to yield a yellow powder characterized by GC/MS as FlSiPh2Cl, i.e. fluorenyl-diphenyl chlorosilane. Crystallization in pentane yields colorless crystals of the product, from which a H-NMR-spectra could be obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05627118 |
|---|
| Source dataset | uspto-grants-1997_05 |
|---|
| ORD ID | ord-9476eff4a94641639478e1b80583b9a4 |
|---|
| Source note | uspto-grants-1997_05 |
|---|