HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 6-Chloropyridine-2,3-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | 6-Chloro-3-nitropyridin-2-ylamine | HCID 2724035 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Water | HCID 962 | — |
| Product | 6-Chloropyridine-2,3-diamine | HCID 10630615 | 86% |
Reaction Steps
4.484 g of iron powder is added to a solution containing 78 ml of acetic acid and 3.415 g of 6-chloro-3-nitro-2-pyridinamine. The reaction medium is heated at 60° C.-70° C. for 2 hours 45 minutes, then left to return to ambient temperature. After pouring into 200 ml of water, 200 ml of ammonium hydroxide is added until pH9 is achieved, followed by extraction with ethyl acetate, drying, filtering and concentrating. 3.14 g of crude product is obtained which is chromatographed on silica eluting with an ethyl acetate triethylamine mixture 95/5. 2.43 g of sought product is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313101B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-2f540a77bafa419c937e038b57f8fec9 |
| Source note | uspto-grants-2001_11 |