HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoromethanesulfonic anhydride → HCID 57454133, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 57452666 | HCID 57452666 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57454133 | HCID 57454133 | 93.1% |
Reaction Steps
N,N-Diisopropylethylamine (0.83 mL, 2 mmol) and trifluoromethanesulfonic anhydride (0.26 mL, 1.6 mmol) were added to a solution of 4-{1-ethyl-1-[4-((E)-3-ethyl-3-hydroxy-1-pentenyl)-3-methyl-phenyl]-propyl}-phenol (Example 39-(3); 0.52 g, 1.4 mmol) in dichloromethane (7 mL) at −78° C., and the mixture was stirred at the same temperature for 10 minutes. A saturated aqueous sodium bicarbonate solution was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=3/1) to give the title compound (0.65 g, 92%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07935688B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-ebe67b9324c540ef891b80f907c4ed16 |
| Source note | uspto-grants-2011_05 |