HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → (3'aR,6'aS)-hexahydro-1'H-spiro(1,3-dioxolane-2,2'-pentalen)-5'-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | HCID 178516323 | HCID 178516323 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | (3'aR,6'aS)-hexahydro-1'H-spiro(1,3-dioxolane-2,2'-pentalen)-5'-one | HCID 11030443 | 31% |
Reaction Steps
cis-Tetrahydropentalene-2,5(1H,3H)-dione (5 g, 36 mmol) and ethylene glycol (2.3 g, 36 mmol) were dissolved in toluene. To the resulting solution was added PTSA (684 mg, 3.6 mmol). The reaction mixture was refluxed for 12 h meanwhile the resulting water was removed away. Direct chromatography on silica gel gave 2.0 g (11 mmol, yield: 31%) of the desired product, (3a′R,6a′S)-tetrahydro-1′H-spiro[1,3-dioxolane-2,2′-pentalen]-5′(3H)-one: MS (m/e): 183 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362003B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-975ff42b56904603a448c685dfa19abf |
| Source note | uspto-grants-2013_01 |