Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | HCID 178455779 | HCID 178455779 | — |
| Reactant | HCID 178455794 | HCID 178455794 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178455778 | HCID 178455778 | 54.4% |
Reaction Steps
In the dichloromethane (50 mL) solution containing 10 g of 2,3-difluoro-4-(trans-4-ethylcyclohexyl)methoxyphenol, 12 g of tripotassium phosphate and 8.1 g of (trans-4-vinylcyclohexyl)methyl methanesulfonate were dissolved, and the solution was stirred at 80 to 100° C. for 2 hours. Water and toluene were added to the solution, and the organic layer was fractioned, washed with water and saturated saline, and then dried over silicagel. The solvent was evaporated under reduced pressure. The residue was purified by recrystallization and column chromatography, to thereby obtain 7.9 g of 2,3-difluoro-1-(trans-4-ethylcyclohexyl)methoxy-4-(trans-4-vinylcyclohexyl)methoxybenzene (1b) in the form of colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08003006B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-6841cf8f44b64655b131b9b248a074c2 |
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| Source note | uspto-grants-2011_08 |
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