HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 66617942, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 945988-97-6 | HCID 66617889 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 66617942 | HCID 66617942 | 45.53% |
Reaction Steps
A flask was charged with ethyl 2-(2-aminopyridin-4-yl)acetate (12.45 g, 69.09 mmol) and acetic acid (100 mL). Bromine (3.550 ml, 69.09 mmol) was added, and the reaction mixture was stirred for 3 hours. The solvent was evaporated in vacuo and the residue was mixed with ice, basified with ammonium hydroxide, and extracted with ethyl acetate. The combined organic layers were washed with brine and concentrated. The residual brown oil was purified by silica gel chromatography, eluting with 1-2% methanol/dichloromethane to provide the desired product (8.15 g, 45.53% yield) as pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022222B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-e39fa3e7cf3240da9cab8a2414608f32 |
| Source note | uspto-grants-2011_09 |