HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → HCID 19434044, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | 3,5-dibromothiophene-2-carbaldehyde | HCID 819040 | — |
| Catalyst | p-Toluenesulfonic acid | HCID 6101 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 19434044 | HCID 19434044 | 81% |
Reaction Steps
A mixture consisting of the product from Step A (11.0 g, 40.7 mmol), TsOH (0.25 g) and ethylene glycol (5.06 g, 81.5 mmol) in toluene (150 mL) was heated at reflux temperature for 1.5 h, water was removed by a Dean-Stark trap. The reaction mixture was cooled and poured into a saturared aqueous solution of sodium bicarbonate (100 mL). The organic layer was separated, dried (MgSO4), and evaporated to dryness. Purification of this crude material by column chromatography (silica, 6% ethyl acetate/hexane) gave 10.33 g of an oil (81%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05538966 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-8d264e1dad26489098f8308b37e4c13c |
| Source note | uspto-grants-1996_07 |