HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → Ethyl 4-(4-oxocyclohexyl)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 2-[4-(1,4-Dioxaspiro[4,5]dec-8-yl)phenyl]-4,4-dimethyl-4,5-dihydro-1,3-oxazole | HCID 59836699 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Ethyl 4-(4-oxocyclohexyl)benzoate | HCID 22633634 | — |
Reaction Steps
3 g of the product of step (iii) (9.51 mmol) are dissolved in 60 ml of ethanol and 4.0 ml of 96% sulphuric acid are added, and the mixture is refluxed for 22 hours. The solvent is partially evaporated off and the remaining mixture is taken up with a mixture of 300 ml of a saturated sodium bicarbonate solution and 150 ml of ethyl acetate. The organic phase is washed with a saturated aqueous NaCl solution. The organic phase is dried and, after filtration, the solvent is evaporated off under reduced pressure. The crude product is purified by chromatography on a silica gel column, eluting with an 8/2 hexane-ethyl acetate mixture. The compound of the title is obtained in the form of a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07419974B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-ace2dad6a97a4a2995806dc716b6302f |
| Source note | uspto-grants-2008_09 |