HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 90416411, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2,4-Difluorophenol | HCID 123051 | — |
| Reactant | HCID 90417779 | HCID 90417779 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 90416411 | HCID 90416411 | 60.1% |
Reaction Steps
A mixture of Example 126B (50 mg, 0.120 mmol), 2,4-difluorophenol (15.62 mg, 0.120 mmol) and cesium carbonate (58.7 mg, 0.180 mmol) in dimethylsulfoxide (0.5 mL) was heated at 120° C. in a microwave oven (Biotage Smith Synthesizer) for 45 minutes. The reaction mixture was partitioned between water and ethyl acetate. The aqueous phase was extracted with ethyl acetate (3×). The combined organic phases were washed with water (2×), saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated and the residue was absorbed on silica gel and purified by flash chromatography (silica gel, 20-90% ethyl acetate/heptanes) to give the title compound (38 mg, 60% yield)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09321764B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-b627ae1fc6f0483ba2d80230ed4eafc5 |
| Source note | uspto-grants-2016_04 |