Hydrochloric Acid → HCID 178418525, compound

Temperature

0 °C

A solution of sodium hypobromide was made by adding Br2 (1.01 ml, 39.5 mmol, 1.1 eq) slowly over a period of 5 min to NaOH (5N, 40 ml) that was previously cooled to 0° C. in an ice bath. The solution was stirred for 10 min before adding 2-hydroxynicotinic acid (5.0 g, 35.9 mmol) and placed in a 50° C. oil bath and stirred. Concurrently, a second pot of sodium hypobromide solution was made by slowly adding Br2 (1.01 ml, 39.5 mmol, 1.1 eq) to a NaOH solution (5N, 40 ml) in an ice bath. The second pot of sodium hypobromide was added to the solution of 2-hydroxynicotinic acid after 24 h of heating then was stirred for an additional 24 h. The solution was cooled to RT, placed in an ice bath and acidified with concentrated HCl while stirring. The precipitate which formed was filtered, washed and dried to afford the desired compound as an off-white solid.

1. customplaced in a 50° C.
2. stirringstirred
3. temperatureof heating
4. stirringthen was stirred for an additional 24 h
5. temperatureThe solution was cooled to RT
6. customplaced in an ice bath
7. stirringwhile stirring
8. customThe precipitate which formed
9. filtrationwas filtered
10. washwashed
11. customdried

ORD record

ord-79764d535c0b47359d2d5159489f4e7e

Source dataset

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08642624B2