HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methane → HCID 57108014, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Nitro-4-(trifluoromethyl)benzoyl chloride | HCID 14323524 | — |
| Reactant | HCID 53912938 | HCID 53912938 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 57108014 | HCID 57108014 | 31.4% |
Reaction Steps
2-nitro-4-trifluoromethylbenzoyl chloride (9.4 g) was added dropwise to a cooled mixture of 1-cyclopropyl-1-diethylaminoethene (5.1 g) and triethylamine (3.7 g) in toluene (100 ml) whilst maintaining the temperature below 10° C. The mixture was then stirred at room temperature for 1 hour. The suspension was treated with decolourising charcoal and filtered. The filtrate was evaporated and the residue was purified by chromatography on silica gel eluted with a mixture of ethyl acetate and dichloromethane (1:9) to give 3-cyclopropyl-3-diethylamino-1-(2-nitro-4-trifluoromethylphenyl)-prop-2-en-1-one (4.1 g) as a red oil with its 1H NMR (in CDCl3) giving peaks at d=0.7-1.8(m, 11H), 3.5(q, 4H), 5.0(s, 1H), 7.5(d, 1H), 7.7(d, 1H),and 7.95(s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05650533 |
| Source dataset | uspto-grants-1997_07 |
| ORD ID | ord-0e52b84397624ce295f50e5e6e9dc26e |
| Source note | uspto-grants-1997_07 |