Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Dichloro(phenyl)silane | HCID 74207 | — |
| Reactant | HCID 178482825 | HCID 178482825 | — |
| Product | HCID 21832787 | HCID 21832787 | 75% |
Reaction Steps
19.87 g (25.8 mmol) of 2,2'-bis(phenyl4-dimethylaminophenyl-phosphinylmethyl)-1,1'-binaphthyl and 15.5 ml (66 mmol) of tributylamine are initially charged in 80 ml of degassed, dry o-xylene in an argon atmosphere while stirring and 9.4 ml (65 mmol) of phenyldichlorosilane are added dropwise. The mixture is subsequently heated at 145° C. for 7 hours while stirring. The reaction mixture is cooled, admixed with 50 ml of degassed 32% strength sodium hydroxide solution and the phases are separated. The organic phase is concentrated and the solid formed is filtered off and recrystallized from acetonitrile. This gives 14.3 g of colorless crystals, corresponding to a yield of 75%.
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-ee21923fb83e4906a6510036950b0811 |
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| Source note | uspto-grants-1998_09 |
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