HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Thiosulfate → 6-Bromo-2,4'-difluoro-3-hydroxybiphenyl 4 carbaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Dibromoisocyanuric acid | HCID 192912 | — |
| Reactant | 2,4'-Difluoro-3-hydroxy-[1,1'-biphenyl]-4-carbaldehyde | HCID 90423951 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 6-Bromo-2,4'-difluoro-3-hydroxybiphenyl 4 carbaldehyde | HCID 90423104 | 122.4% |
Reaction Steps
Dibromoisocyanuric acid (1.49 g) was added at room temperature to a DMF (50 mL) solution of 2,4′-difluoro-3-hydroxybiphenyl-4-carbaldehyde (2.02 g), and the mixture was stirred at the same temperature as above for 3 hours in a nitrogen atmosphere. A saturated aqueous solution of sodium thiosulfate was added to the reaction mixture at room temperature, followed by extraction with ethyl acetate. The obtained organic layer was washed with water and saturated saline in this order and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound (1.99 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09353108B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-44e016c5d39d4ab6a8f5913037987459 |
| Source note | uspto-grants-2016_05 |