Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trichlorosilane | HCID 24811 | — |
| Reactant | HCID 11465546 | HCID 11465546 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 10694978 | HCID 10694978 | 81.2% |
Reaction Steps
7.16 gram (15.2 mmol) of (−)-2-amino-2′-diphenylphosphinyl-1,1′-binaphthyl (the formula (1-1a-1) was dissolved in 381 ml of xylene in an autoclave, followed by the addition of 42.5 ml (305.0 mmol) of triethylamine at 0° C. over 20 minutes and 7.70 ml (76.3 mmol) of trichlorosilane over 1 hour. The mixture was stirred at 150° C. for 18 hours in a tightly sealed condition. The reaction mixture was then extracted with 500 ml of ether. The extract was washed with 200 ml of saturated aqueous solution of ammonium chloride and 200 ml of brine, and then dried over anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure. The residue was purified using a silica gel column chromatography (eluent: 1:4 mixture of ethyl acetate and hexane) to obtain 5.60 gram of the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06323353B1 |
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| Source dataset | uspto-grants-2001_11 |
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| ORD ID | ord-860ba255239b49adba7da33a0aad6e70 |
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| Source note | uspto-grants-2001_11 |
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