HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → Cyclohexanol, 1-ethynyl-, 1-acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 1-Ethynylcyclohexanol | HCID 6525 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Catalyst | Scandium(III) triflate | HCID 2734571 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Cyclohexanol, 1-ethynyl-, 1-acetate | HCID 78903 | 110.7% |
Reaction Steps
To 3.1 g (25 mmol) 1-ethynyl-1-cyclohexanol in 25 ml acetonitrile were added 7.1 ml (75 mmol, 3 eq) acetic anhydride at −20° C. 12.3 mg (0.03 mmol) scandiumtriflate in 300 μl THF were added and the solution was stirred for 2 h. Additional 12.3 mg (0.03 mmol) scandiumtriflate in 300 μl THF were added and stirring was continued for 30 min. A saturated aqueous solution of NaHCO3 and ether were added. The layers were separated and the inorganic one was extracted with ether. The combined organic phases were washed with brine and dried over Na2SO4. Evaporation yielded 4.6 g crude 1-ethynylcyclohexyl acetate as colorless oil, MS: 166 (M).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07449483B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-a67f1e0cc08c4f6a98f30aa3663cf99f |
| Source note | uspto-grants-2008_11 |