HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → HCID 54273351, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | HCID 54197444 | HCID 54197444 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54273351 | HCID 54273351 | 101.9% |
Reaction Steps
4-Nitro-benzenesulfonic acid 4-oxo-tetrahydro-pyran-2-ylmethyl ester (0.5 g, 1.59 mmol), ethylene glycol (986 mg, 15.9 mmol) and p-toluene sulfonic acid (61 mg, 0.32 mmol) were refluxed in benzene (20 ml) for 20 hours. The solvent was removed in vacuo to afford a solid. The solid was dissolved in dichloromethane (30 ml) and successively washed with a saturated aqueous solution of sodium bicarbonate (2×5 ml) and water (2×5 ml). The organic phase was dried (Na2SO4), filtered and the solvent removal in vacuo afforded 582 mg (100%) of 4-nitro-benzenesulfonic acid 1,4,8-trioxa-spiro[4.5]dec-7-ylmethyl ester as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06410586B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-e71ac46cc1774813ae71a60269e6f855 |
| Source note | uspto-grants-2002_06 |