HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → HCID 59773648, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 69220745 | HCID 69220745 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 59773648 | HCID 59773648 | — |
Reaction Steps
250 g of crude 4-(1,4-dioxaspiro[4.5]dec-8-yl)-1-(4-ethoxy-2,3-difluorophenyl)cyclohexan in 1000 ml of toluene are heated on a water separator for 3 h together with 80.0 ml (1.43 mol) of ethylene glycol with addition of 12.0 g (0.06 mol) of p-toluenesulfonic acid monohydrate. After cooling, the batch is washed successively with water, sat. sodium hydrogencarbonate solution and sat. sodium chloride solution. The solution is dried using sodium sulfate and concentrated to dryness. The crude product is crystallised from acetonitrile, giving 8-[4-(4-ethoxy-2,3-difluorophenyl)cyclohex-3-enyl]-1,4-dioxaspiro[4.5]decane as colourless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07417157B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-ae628201f57b4be2873b4a068167ed42 |
| Source note | uspto-grants-2008_08 |