HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-dihydro-2H-pyran → Cyclohexanecarboxylic acid, 4-[(tetrahydro-2H-pyran-2-yl)oxy]-, ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| Reactant | Ethyl 4-hydroxycyclohexanecarboxylate | HCID 86973 | — |
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Cyclohexanecarboxylic acid, 4-[(tetrahydro-2H-pyran-2-yl)oxy]-, ethyl ester | HCID 67249083 | 85% |
Reaction Steps
Pyridinium-4-toluenesulfonate (2.57 g, 10.2 mmol) was added to a solution of ethyl 4-hydroxycyclohexanecarboxylate (8.8 g, 51.10 mmol) and 3,4-dihydro-2H-pyran (8.60 g, 102 mmol) in DCM (200 mL) and the reaction was stirred at rt for 16 h. The reaction was quenched with saturated aq NaHCO3. The layers were separated and the organic layer was washed with water. The organic layer was dried (Na2SO4), filtered, and concentrated. Purification via flash chromatography on a 200 g silica column using an eluent of EtOAc in hexanes (5-10%) afforded the title compound as a clear oil (11.1 g, 85%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08624034B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-59334b9a7bb4486391ffd3835d9cd86d |
| Source note | uspto-grants-2014_01 |