HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methane → HCID 64429773, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Fluoro-2-nitrobenzene | HCID 73895 | — |
| Reactant | 4-Iodopyrazole | HCID 77022 | — |
| Catalyst | Copper oxide | HCID 14829 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 64429773 | HCID 64429773 | 76.2% |
Reaction Steps
A mixture of 1-fluoro-2-nitrobenzene (14.5 g, 0.1 mol), 4-iodopyrazole (20 g, 0.1 mol), potassium carbonate anhydrous (14 g, 0.1 mol) and catalytical amounts of copper(II) oxide in pyridine (35 ml) was heated to reflux for 16 hours. After cooling, the mixture was diluted with dichloromethane (1 litre). Activated charcoal (12 g) was then added and the mixture was heated to reflux for 1 hour. After cooling, it was filtered through celite. The filtrate was evaporated and the remaining oil was purified by silica gel chromatography using ethyl acetate and hexane as eluents, giving 4-iodo-1-(2-nitro-phenyl)-1H-pyrazole (24 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07553798B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-7d6a4bdadb0b4c59a90caaacc71c1312 |
| Source note | uspto-grants-2009_06 |