Hydrochloric Acid → HCID 11673394, compound

To a solution of methyl 2,6-dibromoisonicotinate (10.0 g, 33.91 mmol) in ethanol (200.0 ml) was slowly added NaBH4 (6.4 g, 169.18 mmol) at room temperature under stirring. The reaction was heated to reflux and kept at reflux for 2 hours. The reaction solution was cooled to room temperature, and 2 M HCl (35.0 ml) was added slowly with stirring until the bubbling stopped. The ethanol was removed by rotary evaporation. Solid NaOH was added under stirring until the solution became basic. The solution continued to be stirred, and during stirring the product was precipitated. A white solid product was collected by filtration. After drying, the product was obtained in an amount of 5.0 g (55.6%).

1. customat room temperature
2. temperatureThe reaction was heated
3. temperatureto reflux
4. temperatureat reflux for 2 hours
5. stirringwith stirring until the bubbling
6. customThe ethanol was removed by rotary evaporation
7. additionSolid NaOH was added
8. stirringunder stirring until the solution
9. stirringto be stirred
10. stirringduring stirring the product
11. customwas precipitated
12. filtrationA white solid product was collected by filtration
13. customAfter drying
14. customthe product was obtained in an amount of 5.0 g (55.6%)

ORD record

ord-5ced20bc251c4bccbec60065cfdd784c

Source dataset

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08546505B2