HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 58158548, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 5-Chloro-2-nitropyridine | HCID 259806 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 58158634 | HCID 58158634 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58158548 | HCID 58158548 | 83% |
Reaction Steps
To a solution of benzyl (3-fluoro-4-hydroxyphenyl)carbamate (80 g, 252 mmol) in dimethyl sulfoxide (600 mL) were added cesium carbonate (123 g, 378 mmol) and 5-chloro-2-nitropyridine (40 g, 252 mmol), and the mixture was stirred at room temperature for 3 hr. Saturated aqueous sodium hydrogen carbonate (1000 mL) and water (1000 mL) were added to the reaction mixture, and the mixture was extracted twice with ethyl acetate. The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered. The solvent was evaporated under reduced pressure, and the residue was washed with hexane/ethyl acetate (=3/1) and collected by filtration to give the title compound (79.8 g, 83%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08445509B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-24ec7688bb4c4f1e9b2fa9507fde4560 |
| Source note | uspto-grants-2013_05 |