Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Chlorodiphenylphosphine | HCID 66180 | — |
| Reactant | HCID 15621733 | HCID 15621733 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18424475 | HCID 18424475 | 66.1% |
Reaction Steps
Into a reactor were introduced 2.00 g (6.00 mmol) of the 1,1-bis(4-methoxyphenyl)-2-bromopropene and 30 mL of THF under a nitrogen atmosphere. The contents were cooled to −65° C., and 4.0 mL (6.0 mmol; 1.5 M hexane solution) of butyllithium was gradually added dropwise thereto. The resultant mixture was stirred for 30 minutes. Thereafter, 0.90 mL (5.0 mmol) of chlorodiphenylphosphine was added, and this mixture was stirred at that temperature for 1 hour and then at room temperature for 1 hour. Saturated aqueous ammonium chloride solution was added to the reaction mixture. The resultant mixture was extracted with ethyl acetate, and the extract was dried with anhydrous magnesium sulfate. Thereafter, the solvent was removed under reduced pressure. The concentrate was recrystallized from ethanol to obtain 1.45 g (66%) of the target compound as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06455720B1 |
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| Source dataset | uspto-grants-2002_09 |
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| ORD ID | ord-576775abf16c443d985114e4973313d5 |
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| Source note | uspto-grants-2002_09 |
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