HuagongsheHuagongshe Chemistry Print Report · For research reference only
8-(3-Hydroxy-3-(p-tolyl)propyn-1-yl)-1,4-dioxaspiro[4.5]decan-8-ol → 3-(8-Hydroxy-1,4-dioxaspiro[4.5]decan-8-yl)-1-(p-tolyl)-2-propyn-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 8-(3-Hydroxy-3-(p-tolyl)propyn-1-yl)-1,4-dioxaspiro[4.5]decan-8-ol | HCID 58399358 | — |
| Catalyst | HCID 178418406 | HCID 178418406 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-(8-Hydroxy-1,4-dioxaspiro[4.5]decan-8-yl)-1-(p-tolyl)-2-propyn-1-one | HCID 58399381 | 82.2% |
Reaction Steps
To a solution of 8-(3-hydroxy-3-(p-tolyl)propyn-1-yl)-1,4-dioxaspiro[4.5]decan-8-ol (Reference Example 3) (17.5 g, 57.9 mmol) in dichloromethane (289 mL), manganese dioxide (29.6 g, 289 mmol) was added, and the obtained solution was stirred at room temperature for 15 hours. The reaction solution was filtered through Celite and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography (silica gel, n-hexane/ethyl acetate) to obtain the captioned compound (14.3 g, 47.6 mmol, 82%) as an oily product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247569B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-af7cf1072fa94858ad40e44d0e06b9c4 |
| Source note | uspto-grants-2012_08 |