HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyldichlorosilane → 2,2'-Bis((diphenylphosphaneyl)methyl)-1,1'-binaphthalene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyldichlorosilane | HCID 6376 | — |
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | 2,2'-Bis(diphenylphosphinylmethyl)-1,1'-binaphthyl | HCID 10952532 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | 2,2'-Bis((diphenylphosphaneyl)methyl)-1,1'-binaphthalene | HCID 10952407 | — |
Reaction Steps
409.7 g (0.6 mol) of 2,2'-bis(diphenylphosphinylmethyl)-1,1'-binaphthyl are suspended in 1.5 1 of xylene and 715 ml (3.0 mol) of tri-n-butylamine in the absence of air and moisture, and 345.1 g (3.0 mol) of methyldichlorosilane are added dropwise with stirring. The mixture is then refluxed for 12 hours to give a clear solution. Xylene is distilled off at atmospheric pressure, and the mixture is allowed to cool with stirring. This results in the formation of 2,2'-bis(diphenylphosphinomethyl)-1,1'-binaphthyl as a colorless solid, which is filtered off under an inert gas and washed with 200 ml of degassed acetone. 378 g (97%) of colorless crystals of melting point 160° to 161° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05600006 |
| Source dataset | uspto-grants-1997_02 |
| ORD ID | ord-bd35cf771f5b46d3a4a0ab09e3c12849 |
| Source note | uspto-grants-1997_02 |