HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 1279815-28-9
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 4,6-Dichloronicotinamide | HCID 600044 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 1279815-28-9 | HCID 118598557 | — |
Reaction Steps
To a well stirred solution of 4,6-dichloropyridine-3-carboxamide (11.0 g, 57.59 mmol) in 1,4-dioxane (20 mL) in steel bomb was added the liquid ammonia (50 mL, 57.59 mmol). The steel bomb was closed and heated the reaction to 100° C. for 9 h. The progress of the displacement reaction was monitored by TLC and LCMS. After completion the solid formed was filtered. The filtrate was also concentrated as it also contains 50% product. The combined solids were dried under vacuum to afford 4-amino-6-chloro-pyridine-3-carboxamide (2) as a light brown solid. Yield: 10.6 g, crude, 47%; 1H NMR (400 MHz, DMSO-d6) δ 8.36 (s, 1H), 7.97 (s, 1H), 7.50 (s, 1H), 7.37 (s, 1H), 6.65 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09382248B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-29bf2b56551a4d088895cfde1c9247ad |
| Source note | uspto-grants-2016_07 |