HuagongsheHuagongshe Chemistry Print Report · For research reference only
Calcium Chloride → HCID 178507679, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Calcium Chloride | HCID 5284359 | — |
| Reactant | HCID 178526657 | HCID 178526657 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178507679 | HCID 178507679 | 71.3% |
Reaction Steps
To an 80% aqueous ethanol suspension (150 ml) of 5-chloro-3-nitropyridin-2-ol (15.0 g) and calcium chloride (9.54 g) was added iron powder (24.0 g), followed by stirring at room temperature for 30 minutes, and further under heating at reflux for 1 hour. After the temperature was brought back to room temperature, the reaction suspension was filtered through Celite. Water was added to the filtrate, and extracted 8 times with a methanol-dichloromethane (1:10) mixed solvent. The collected organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure to afford 3-amino-5-chloropyridin-2-ol (8.86 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08729095B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-3d84b51c89c04dcdb4b987d199d70681 |
| Source note | uspto-grants-2014_05 |