HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine → 3,5-Dichloro-2-hydrazinylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | Pyridine, 2,3,5-trichloro- | HCID 27666 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 3,5-Dichloro-2-hydrazinylpyridine | HCID 600966 | 72% |
Reaction Steps
To a 500 mL flask, 2,3,5-trichloropyridine (20.00 g, 0.110 mol), 80% hydrazine (34.30 g, 0.550 mol) and dioxane (200 mL) were added sequentially. The reaction mixture was heated to reflux for 20 hours. Then the reaction mixture was cooled down to room temperature overnight and white crystal was precipitated. The white crystal was isolated via filtration and dried to give the product (14.0 g) as a white solid in 72% yield. Melting point: 187-189° C. 1H NMR (300 MHz, DMSO-d6): 8.123 (d, 1H), 7.849 (d, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08492409B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-77228aae130a4fbbaf2bddb21c1687bb |
| Source note | uspto-grants-2013_07 |