HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → (2-Nitrophenyl)-terephthalamic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2-Nitroaniline | HCID 6946 | — |
| Reactant | Methyl 4-(chlorocarbonyl)benzoate | HCID 81850 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | (2-Nitrophenyl)-terephthalamic acid methyl ester | HCID 68619015 | 78% |
Reaction Steps
A solution of 2-nitroaniline (0.41 g, 3.0 mmol) and methyl 4-chlorocarbonyl benzoate (0.65 g, 3.3 mmol) in THF (3.7 mL) and pyridine (0.8 mL) was stirred for 2 h at room temperature. The reaction was diluted with saturated sodium bicarbonate (10 mL) and EtOAc (15 mL), the phases separated and the aqueous phase extracted with EtOAc (2×10 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated under reduced pressure to afford (2-nitrophenyl)-terephthalamic acid methyl ester as a yellow solid (0.70 g, 78%). 1H NMR (CDCl3) δ 3.97 (s, 3H), 7.25 (t, 1H, J=7.8 Hz), 7.74 (t, 1H, J=7.8 Hz), 8.04 (d, 2H, J=7.8 Hz), 8.20 (s, 1H (NH)), 8.20 (d, 2H, J=7.8 Hz), 8.30 (d, 1H, J=7.8 Hz), 8.99 (d, 1H, J=7.8 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07807694B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-061122d744b84005bbf381650095037c |
| Source note | uspto-grants-2010_10 |