Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Benzene, 1-bromo-4-(trifluoromethyl)- | HCID 67872 | — |
| Reactant | 4-Fluoro-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline | HCID 23152508 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 54912257 | HCID 54912257 | — |
Reaction Steps
Under argon, a mixture of 9.0 g (37.9 mmol) of 4-fluoro-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline, 10.25 g (45.5 mmol) of 4-bromobenzotrifluoride, 1.39 g (1.89 mmol) of 1,1′-bis(diphenyl-phosphino)ferrocenepalladium(II) chloride and 20.11 g (189 mmol) of sodium carbonate in 200 mL of DMSO and 70 mL of water is stirred at 90° C. overnight. After the reaction has ended, the mixture is cooled to room temperature, water is added and the mixture is extracted with ethyl acetate. The organic phase is once more washed with water, dried with sodium sulfate and concentrated under reduced pressure. The crude product is purified by column chromatography (mobile phase: cyclohexane/ethyl acetate gradient). This gives 5.28 g (53% of theory) of 5-fluoro-4′-(trifluoromethyl)biphenyl-2-amine having a content of 97% according to LC-MS and a logP (acidic) of 3.52.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09375004B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-ef835d7f76894537b73e6bf1ea6026fd |
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| Source note | uspto-grants-2016_06 |
|---|