HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 11120552, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,4-Dioxaspiro[4.5]decan-8-one | HCID 567415 | — |
| Reactant | HCID 86678943 | HCID 86678943 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11120552 | HCID 11120552 | 94.8% |
Reaction Steps
To a solution of 1,4-dioxaspiro[4.5]decan-8-one (11.6 g) in dichloromethane (200 mL) were added dropwise triethylamine (20.7 mL) and trifluoromethyl tri(propan-2-yl)silyl sulfate (25.0 g). The reaction mixture was stirred at room temperature so for 1 hr, and ice-cooled water was added. The organic layer was separated, washed with water and saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/petroleum ether) to give the title compound (22.0 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772277B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-ff1754c165814ece8533542c8bd06767 |
| Source note | uspto-grants-2014_07 |