HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine → HCID 178434352, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | 1-(2,4-Dichloropyridin-3-yl)ethan-1-one | HCID 53402442 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178434352 | HCID 178434352 | 64% |
Reaction Steps
1-(2,4-Dichloro-pyridin-3-yl)-ethanone (6.2 g, 32.6 mmol) in 65% aqueous hydrazine (45 ml) was stirred at rt overnight. The mixture was diluted with EtOAc and water. The organic extract was washed with brine, dried and concentrated to give a white solid. The crude product was purified by flash column chromatography over silica gel (200 g) eluting with 1:1 petroleum ether:EtOAc to give an off-white solid (3.5 g, 64%). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.64 (s, 3 H), 7.47 (d, J=5.95 Hz, 1 H), 8.06 (d, J=5.95 Hz, 1 H). m/z (ES+APCI)+: 168/170 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08569281B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-039190ea76dc41b2ab4f71516e2c9086 |
| Source note | uspto-grants-2013_10 |