HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 3-(4-Chloro-2-iodophenylamino)cyclohex-2-enone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1,3-Cyclohexanedione | HCID 10434 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | 4-Chloro-2-iodoaniline | HCID 2757615 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 3-(4-Chloro-2-iodophenylamino)cyclohex-2-enone | HCID 67328785 | 80.7% |
Reaction Steps
A mixture of 4-chloro-2-iodoaniline (0.5 g, 1.97 mmol), 1,3-cyclohexanedione (0.22 g, 1.96 mmol) and p-toluenesulfonic acid monohydrate (catalytic) in toluene (6 mL) were heated to reflux for 2 h. The reaction was cooled and EtOAc (50 mL) was added and the organic phase was washed with water (20 mL) and brine (20 mL), dried over sodium sulfate, filtered and evaporated to give a brown solid, which was purified by column chromatography [Silica, eluent: EtOAc:hexane to give 3-(4-chloro-2-iodophenylamino)cyclohex-2-enone as a yellow solid (0.55 g, 80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09199985B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-fa2d5edb06834aa7a1d49ba7cb7cd1d4 |
| Source note | uspto-grants-2015_12 |