Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 86710069 | HCID 86710069 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89954219 | HCID 89954219 | 98.4% |
Reaction Steps
{3-(4,4-Difluorocyclohexyl)-1-(1-trifluoromethylcyclopropyl)prop-1-enyloxy}triethylsilane (3.00 g, 7.53 mmol) obtained in step 4 was dissolved in dichloromethane (30 mL). Under ice-cooled condition, a dichloromethane solution (10 mL) of bromine (1.32 g, 8.28 mmol) was added, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was extracted with hexane after adding a saturated sodium hydrogen carbonate aqueous solution, and a sodium thiosulfate aqueous solution. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=90/10→80/20) to give 2-bromo-3-(4,4-difluorocyclohexyl)-1-(1-trifluoromethylcyclopropyl)propan-1-one (2.69 g, yield 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09000186B2 |
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| Source dataset | uspto-grants-2015_04 |
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| ORD ID | ord-0555b317194c47d38a9cd09beaf74cfe |
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| Source note | uspto-grants-2015_04 |
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