Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hexachloroethane | HCID 6214 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 66961793 | HCID 66961793 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66961006 | HCID 66961006 | 72.7% |
Reaction Steps
To a THF (50 mL) solution of 1-(4-[1,3]dioxolan-2-yl-2-methoxyphenyl)-1H-imidazole (3.85 g), n-butyllithium (1.6M hexane solution, 12 mL) was added dropwise under nitrogen atmosphere at −78° C., and the reaction solution was agitated for 30 minutes. THF (10 mL) solution of hexachloroethane (6.1 g) was added to the reaction solution and the reaction solution was agitated at room temperature for 1 hour after agitating for 30 minutes at −78° C. Water and ethyl acetate were added to the reaction mixture, and the organic layer was partitioned. The organic layer was washed with a saturated saline solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent:hexane-ethyl acetate system), and 3.19 g of the title compound was obtained. The physical properties of the compound are as follows.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07667041B2 |
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| Source dataset | uspto-grants-2010_02 |
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| ORD ID | ord-985fdd40f5ec42279b8360c6b63a27cb |
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| Source note | uspto-grants-2010_02 |
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