Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 178418543 | HCID 178418543 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178418525 | HCID 178418525 | 78% |
Reaction Steps
To a suspension of 5.0 g (35.9 mmol) of 2-hydroxy-nicotinic acid in 30 ml acetic acid was added dropwise 7.5 g (46.7 mmol) bromine. The mixture was maintained at 70-80° C. overnight. The mixture was cooled and the acetic acid was removed under reduced pressure. Water (100 ml) was added and the product was filtered and washed with water (3×100 ml). The solid was dried in a vacuum oven at 65° C. for 48 hours to provide 6.1 g (78% yield) of the title compound. MS: m/z (APCI, AP+) 219.0 [M.]+. CHN Analysis: Calcd: C, 33.06; H, 1.85; N, 6.42. Found: C, 32.91; H, 1.78; N, 6.23.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06881743B2 |
|---|
| Source dataset | uspto-grants-2005_04 |
|---|
| ORD ID | ord-55eeab62b52247ba9bac5c1a45d6513f |
|---|
| Source note | uspto-grants-2005_04 |
|---|