Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl Acrylate | HCID 7294 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Tri-o-tolylphosphine | HCID 80271 | — |
| Reactant | 2-Bromo-4-trifluoromethylaniline | HCID 93899 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 15453700 | HCID 15453700 | 36.5% |
Reaction Steps
A 100 ml 3-neck flask with magnetic stirrer was charged with 2-bromo-4-(trifluoromethyl)aniline (500 mg, 2.08 mmol), methyl acrylate (538 mg, 6.25 mmol), Pd(OAc)2 (23.3 mg, 0.104 mmol), P(o-tolyl)3 (64 mg, 0.21 mmol), triethylamine (422 mg, 4.7 mmol) and acetonitrile (20 ml). The flask was purged with N2 and heated to 90° C. overnight. Saturated aqueous NH4Cl (40 ml) was added, and the mixture was extracted with ethyl acetate (10 ml*3). The organic layer was dried over Na2SO4, filtered, and concentrated to dryness. The crude product was purified by silica gel chromatography to give (E)-methyl 3-(2-amino-5-(trifluoromethyl)phenyl)acrylate (185.9 mg, 36.5%) as a yellow solid. 1H NMR (400 MHz, CDCl3) δ 7.69 (d, J=16 Hz, 1H), 7.53 (s, 1H), 7.32 (d, J=8.8 Hz, 1H), 6.67 (d, J=8.8 Hz, 1H), 6.34 (d, J=16 Hz, 1H), 4.20 (s, 2H), 3.74 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09139538B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-7f6c3e1d09674e03b20ce88e1e61bb54 |
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| Source note | uspto-grants-2015_09 |
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