HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → 5-Bromo-N3-[1-(tetrahydro-2H-pyran-4-yl)ethyl]pyridine-2,3-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 5-Bromopyridine-2,3-diamine | HCID 691156 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 1-(Tetrahydro-2H-pyran-4-yl)ethanone | HCID 9877365 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 5-Bromo-N3-[1-(tetrahydro-2H-pyran-4-yl)ethyl]pyridine-2,3-diamine | HCID 86652369 | 19.6% |
Reaction Steps
2,3-Diamino-5-bromopyridine (1.07 g) and 1-(tetrahydro-2H-pyran-4-yl)ethanone (0.80 g) were dissolved in methanol (20 ml), and acetic acid (0.98 ml) was added. After stirring at room temperature for a while, sodium cyanoborohydride (1.08 g) was added and the mixture was stirred at room temperature for 20 hours. A saturated aqueous sodium bicarbonate solution was added to the reaction solution, followed by extraction with ethyl acetate. Then, the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The resulting residue was purified by flash column chromatography (developed with ethyl acetate-hexane) to give the title compound (334 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785438B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-14c64c082ffb43ca93d362306b63ca45 |
| Source note | uspto-grants-2014_07 |