HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 70872693, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 5-Bromo-4,6-dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile | HCID 737752 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 70872693 | HCID 70872693 | 94% |
Reaction Steps
To a stirred solution of 5-bromo-4,6-dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile (1 g, 4.44 mmol) and NiCl2.6H2O (0.21 g, 0.89 mmol) in methanol at 0° C., NaBH4 (0.68 g, 17.78 mmol) was added portion wise. Reaction mixture was then stirred at rt for overnight period. On completion, it was acidified using 3N HCl and stirred at rt for 3 h. Solvent was removed under reduced pressure. Residue was washed with diethyl ether and basified with aq. NH4OH. Compound was extracted in 10% MeOH in DCM and dried over anhydrous Na2SO4 to give the title compound (0.96 g, 94%) which was used as such for coupling reaction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08765732B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-94527e69b7b2463989b5355be62b4e9d |
| Source note | uspto-grants-2014_07 |