HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiophenol → Ethyl 3-oxo-4-(phenylthio)cyclohexanecarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Ethyl 4-bromo-3-oxocyclohexanecarboxylate | HCID 12917736 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Ethyl 3-oxo-4-(phenylthio)cyclohexanecarboxylate | HCID 58999613 | 61.3% |
Reaction Steps
To a solution of ethyl 4-bromo-3-oxocyclohexanecarboxylate (3.73 g, 15 mmol) in EtOH (30 mL) at 80° C. was added a solution of benzenethiol (1.65 mL, 15 mmol) and NaOH (0.6 g, 15 mmol) in EtOH (100 mL). The suspension was stirred for 1 hour, then was concentrated in vacuo. The residue was diluted with water and extracted with EtOAc. The organic layer was washed with water then brine, then was dried over MgSO4 and concentrated in vacuo. Purification by chromatography on silica gel afforded 2.56 g (61%) of the title compound as a yellow oil: MS (−) 277 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07297704B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-5fe8248b5ef84d848efa74c3fdf50697 |
| Source note | uspto-grants-2007_11 |