Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | Dichloro(phenyl)silane | HCID 74207 | — |
| Reactant | HCID 21832791 | HCID 21832791 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 21832792 | HCID 21832792 | 95% |
Reaction Steps
12.0 g (19.5 mmol) of 1,3-bis[bis(4-dimethylaminophenyl)phosphinyl]propane and 24 ml (100 mmol) of tri-n-butylamine are initially charged in 80 ml of o-xylene in an argon atmosphere while stirring. 14.4 ml (100 mmol) of phenyldichlorosilane are slowly added dropwise. The mixture is heated to 145° C., stirred for 6 hours and the solvent is distilled off under reduced pressure. Cooling the clear solution results in formation of colorless crystals which are filtered off. The crystals obtained are suspended in 100 ml of degassed o-xylene and extracted with 20 ml of 2N sodium hydroxide solution. The organic phase is separated off, dried with sodium sulphate and evaporated under reduced pressure. This gives 10.8 g of colorless solid, corresponding to a yield of 95%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05801287 |
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| Source dataset | uspto-grants-1998_09 |
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| ORD ID | ord-2014a5eb3ca84d5c96e02a18bcad85be |
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| Source note | uspto-grants-1998_09 |
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