HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 79458467, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,3-Cyclohexanediamine | HCID 18814 | — |
| Reactant | 1-Fluoro-2-nitrobenzene | HCID 73895 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 79458467 | HCID 79458467 | 49.3% |
Reaction Steps
To a suspension of 2-fluoronitrobenzene (197 mg) and potassium carbonate (193 mg) in acetonitrile (4 mL), 1,3-cyclohexanediamine (480 mg) was added at room temperature, and the mixture was stirred for 10 hours and 30 minutes under reflux by heating. The reaction mixture was cooled to room temperature, and then ethyl acetate and water were added to the reaction mixture. The organic layer was separated, washed with saturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (eluent, 100 to 80% ethyl acetate in methanol) to obtain N1-(2-nitrophenyl)cyclohexane-1,3-diamine (C41, 162 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145415B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-4320526ea24a4385aec9c729a7216a17 |
| Source note | uspto-grants-2015_09 |