HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 3-Fluoro-4-(4-methylpiperazin-1-yl)benzene-1,2-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | 2-Fluoro-3-(4-methyl-piperazin-1-yl)-6-nitro-phenylamine | HCID 22040816 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 3-Fluoro-4-(4-methylpiperazin-1-yl)benzene-1,2-diamine | HCID 22040743 | — |
Reaction Steps
A 25 mL round bottom flask was charged with a suspension of 1 (600 mg, 2.2 mmol), methoxylamine HCl (202 mg, 2.42 mmol), and pyridine (0.22 mL, 2.6 mmol) in ethanol (9 mL). The resulting reaction mixture was stirred at rt overnight. The crude product was concentrated, absorbed onto silica gel, and purified by flash chromatography (97:3 CH2Cl2/MeOH) to give 2 as an orange solid. LCMS m/z 303.2 (MH+), tR=2.40 mm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08614330B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-a69bf5bdac2343ed806a51e542955c92 |
| Source note | uspto-grants-2013_12 |