HuagongsheHuagongshe Chemistry Print Report · For research reference only
8-(3-Fluorophenyl)-1,4-dioxaspiro[4.5]dec-7-ene → 8-(3-Fluorophenyl)-1,4-dioxaspiro[4.5]decane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 8-(3-Fluorophenyl)-1,4-dioxaspiro[4.5]dec-7-ene | HCID 18787932 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 8-(3-Fluorophenyl)-1,4-dioxaspiro[4.5]decane | HCID 18787926 | — |
Reaction Steps
The compound (17) was dissolved in a mixed solvent of toluene (150 ml) and Solmix (150 ml) and 3.48 g of Pd/C was added thereto. The mixture was stirred at room temperature under a hydrogen atmosphere until hydrogen absorption had ceased. After the reaction had been completed, Pd/C was removed and then the solvent was distilled off. The residue was purified with a fractional operation by means of column chromatography using a mixed solvent of toluene and ethyl acetate (toluene:ethyl acetate=9:1 by volume) as an eluent and silica gel as a stationary phase powder and dried, giving 61.9 g of 8-(3-fluorophenyl)-1,4-dioxaspiro[4,5]decane (18). The yield based on the compound (17) was 88.1%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08137583B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-54864268b135497891ac8bf95a3dc1be |
| Source note | uspto-grants-2012_03 |