HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → HCID 18673916, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- | HCID 18462 | — |
| Reactant | HCID 17405231 | HCID 17405231 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 18673916 | HCID 18673916 | — |
Reaction Steps
380 mg of 1-{4-[(5-nitro-2-pyridinyl)oxy]phenyl}-1-ethanone was dissolved in 5 ml of benzene and, after adding 98 μl of ethylene glycol and 3 mg of (±)-10-camphorsulfonic acid, the mixture was heated at reflux. After 3 hours, the reaction solution was extracted with ethyl acetate. The organic layer was washed in turn with a saturated sodium hydrogencarbonate solution and a saturated sodium chloride solution, dried over magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (eluent: ethyl acetate/n-hexane (1:4)) to obtain the titled compound (280 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06511995B1 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-10197552adcd402ab1d40ce6e08bb0dd |
| Source note | uspto-grants-2003_01 |