HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 15462861, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 4-Methylcyclohexanone | HCID 11525 | — |
| Reactant | 1-Methyl-3,5-dinitro-1H-pyridin-2-one | HCID 3621236 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 15462861 | HCID 15462861 | 73% |
Reaction Steps
4-Methylcyclohexanone (170 mg, 1.52 mmol) was mixed with 1-methyl-3,5-dinitro-2-pyridone (300 mg, 1.51 mmol) in 1M methanolic ammonia (30 mL, 30 mmol). The solution was heated at gentle reflux for 3 h. Evaporation of the solvent gave an orange residue which was suspended in CHCl3 and flash chromatographed over silica gel (16 g) eluting with EtOAc/hexane (1:10) to afford a white solid (211 mg, 73% yield): mp 50°-52° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05866579 |
| Source dataset | uspto-grants-1999_02 |
| ORD ID | ord-248af8e751054f88bb128f9377438adf |
| Source note | uspto-grants-1999_02 |