Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Iodine | HCID 807 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 68714689 | HCID 68714689 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68714169 | HCID 68714169 | — |
Reaction Steps
To a stirred solution of triphenylphosphine (1.56 g, 6.0 mmol) and imidazole (0.41 g, 6.0 mmol) in dichloromethane (16 ml) under an argon atmosphere was added slowly iodine (1.51 g, 6.0 mmol) and 2-(3-chloro-phenyl)-5,5,5-trifluoro-pentan-1-ol (1.26 g, 5.0 mmol). The mixture was stirred for 2 hours at room temperature, then dichloromethane (50 ml) was added and mixture was extracted with saturated sodium thiosulfate solution (50 ml) and hydrochloric acid (1N, 25 ml). The organic layer was dried over MgSO4 and evaporated. The residue was suspended in ether and filtered to remove insoluble triphenylphosphine oxide. The ether was evaporated and the residue was purified by column chromatography (SiO2, heptane/EtOAc=9:1) to yield a light yellow liquid, (1.73 g, 96%); (EI): 235.0 ((M−I)+.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08604061B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-74a42f2d2adc4718ade96dea61b30e84 |
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| Source note | uspto-grants-2013_12 |
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