HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 3785006, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Aniline | HCID 6115 | — |
| Reactant | 2,6-Dichloro-3-nitropyridine | HCID 85239 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 3785006 | HCID 3785006 | — |
Reaction Steps
2,6-dichloro-3-nitropyridine (II-1, 193 mg, 1 mmol), phenylamine (III-2, 93 mg, 1 mmol) and sodium bicarbonate (84 mg, 1 mmol) were added to 10 mL anhydrous ethanol, and reacted at room temperature for 24 h. The reaction solution was poured into ice water, and adjusted with diluted HCl to a pH of 5-6, followed by stirring for 30 min, to precipitate a solid. The solid was filtered out, washed with water until neutral, and then dried to obtain compound IV-2 (219 mg, 88), a red solid, mp 95-98° C. 1H NMR (CDCl3) δ 10.28 (1H, b s, NH), 8.47 (1H, d, J=8.4 Hz, ArH-4), 7.66 (2H, d, J=8.0 Hz, ArH-2′, 6′), 7.42 (2H, t, J=8.0 Hz, ArH-3′, 5′), 7.21 (1H, t, J=7.2 Hz, ArH-4′), 6.81 (1H, d, J=8.4 Hz, ArH-5); MS (m/z): 250 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08933106B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-89f872d609074dcb8155579bf364bc73 |
| Source note | uspto-grants-2015_01 |