Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium fluoride | HCID 25953 | — |
| Reactant | 2-(Trifluoromethyl)benzeneboronic acid | HCID 2734387 | — |
| Reactant | Methyl 4-bromo-3-(methoxymethyl)benzoate | HCID 58554220 | — |
| Reactant | 2-Dicyclohexylphosphino-2,6-dimethoxybiphenyl | HCID 66545337 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 66718285 | HCID 66718285 | — |
Reaction Steps
A mixture of methyl 4-bromo-3-(methoxymethyl)benzoate (Intermediate 1 Step 2, 8.0 g, 30.8 mmol), 2-(trifluoromethyl)phenylboronic acid (8.8 g, 46.3 mmol), cesium fluoride (14.0 g, 92.4 mmol), palladium acetate (0.69 g, 3.1 mmol) and 2-dicyclohexylphosphino-2,6-dimethoxybiphenyl (3.16 g, 7.7 mmol) was prepared in a mixture of dioxane (80 mL) and water (80 mL) under nitrogen atmosphere and heated at 100° C. for 12 hours. The reaction mixture was concentrated under vacuum. The residue was diluted with EtOAc (200 mL), and then washed with water (100 mL) and brine (100 mL). The organic layer was dried (Na2SO4) and concentrated under vacuum. After purification by flash chromatography (silica, pet ether/EtOAc), the title compound was obtained as a pale yellow solid (8.0 g, 88%). 1H NMR (CDCl3, 400 MHz) δ 8.22 (1H, s), 7.99 (1H, d, J=6.5 Hz), 7.78 (1H, d, J=7.7 Hz), 7.57 (2H, m), 7.27 (2H, m), 4.19-4.10 (2H, m), 3.95 (3H, s), 3.26 (3H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08802704B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-978b06dc5c5b4b30a1bb62053335fba7 |
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| Source note | uspto-grants-2014_08 |
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