HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → HCID 68683108, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | 3,5-Difluoropropiophenone | HCID 145620 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68683108 | HCID 68683108 | 98.2% |
Reaction Steps
Ethylene glycol (773 mg) and a catalytic amount of tosylic acid monohydrate were added to a toluene (20 ml) solution of 1-(3,5-difluorophenyl)propan-1-one (1.06 g). A Dean-Stark tube was attached to the reactor, the reaction liquid was stirred overnight with heating under reflux, then diluted with ethyl acetate, and washed with aqueous saturated sodium hydrogencarbonate solution. The organic layer was dried with anhydrous sodium sulfate, then the solvent was evaporated off, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1) to obtain the entitled compound (1.31 g) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07829586B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-5b0085f2a3e14012a357edb48fa2e3c0 |
| Source note | uspto-grants-2010_11 |