HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → 4-Bromo-3-(1,3-dioxolan-2-yl)-2-fluorophenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 6-Bromo-2-fluoro-3-hydroxybenzaldehyde | HCID 53438799 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4-Bromo-3-(1,3-dioxolan-2-yl)-2-fluorophenol | HCID 67440478 | 94% |
Reaction Steps
A solution of 6-bromo-2-fluoro-3-hydroxybenzaldehyde (1.61 g, 7.35 mmol), ethylene glycol (2 mL, 36.8 mmol), para-toluenesulfonic acid (0.27 g, 0.147 mmol), and toluene (150 mL) was refluxed with a dean-stark head for 16 hours. An aqueous solution of sodium bicarbonate was added and the solution was extracted with ethyl acetate. The aqueous layer was extracted five more times with ethyl acetate. The organic layers were combined and washed with brine, dried over anhydrous sodium sulfate, and filtered. The solvent was removed under reduced pressure to give 4-bromo-3-(1,3-dioxolan-2-yl)-2-fluorophenol (1.81 g, 94% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09416146B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-9b0a8321d5e64425ab6d184fd8b6b20d |
| Source note | uspto-grants-2016_08 |