HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 6-Methylpyridine-2,4-diol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | 4-Hydroxy-6-methyl-2-pyrone | HCID 54675757 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 6-Methylpyridine-2,4-diol | HCID 54691419 | 88% |
Reaction Steps
4-Hydroxy-6-methyl-2H-pyran-2-one (11.1 g, 88.0 mmol) was suspended into ethanol (5.0 mL), added with 28% aqueous ammonia (55 mL), and the resultant mixture was stirred at 100° C. for 1 hour. The reaction solution was cooled down to room temperature, added with chloroform (25 mL) and ether (25 mL) to extract solid substance which was then washed sequentially with chloroform (10 mL), ether (10 mL) and tetrahydrofuran (30 mL), and concentrated in vacuo. Then, the obtained residue was further washed sequentially with chloroform (10 mL), ether (10 mL) and tetrahydrofuran (30 mL). 4-Hydroxy-6-methylpyridin-2(1H)-one (9.70 g, yield 88%) was obtained as a pale yellow crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08153634B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-d6b7cef893fc40af88ac0caeb5558632 |
| Source note | uspto-grants-2012_04 |