Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trichlorosilane | HCID 24811 | — |
| Reactant | HCID 12010732 | HCID 12010732 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 15504838 | HCID 15504838 | 87.9% |
Reaction Steps
3.93 gram (7.17 mmol) of (−)-2-methylsulfonylamino-2′-diphenylphosphinyl-1,1′-binaphthyl (the formula (1-3a-1)) was dissolved in 179 ml of xylene in an autoclave, followed by the addition of 20.0 ml (143.4 mmol) of triethylamine at 0° C. over 15 minutes and 3.62 ml (35.8 mmol) of trichlorosilane over 30 minutes. The mixture was stirred at 150° C. for 18 hours in a tightly sealed condition. The reaction mixture was then extracted with 300 ml of ether. The extract was washed with 100 ml of saturated aqueous solution of ammonium chloride and 100 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: 1:6 mixture of ethyl acetate and hexane) to obtain 3.35 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-e6fbd90fce3944728d7b0a4f343eeeb2 |
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| Source note | uspto-grants-2001_11 |
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