HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 68630898, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | (2-Amino-pyridin-3-yl)-pyridin-3-yl-methanone | HCID 53678495 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 68630898 | HCID 68630898 | — |
Reaction Steps
(2-Amino-pyridin-3-yl)-pyridin-3-yl-methanone (0.13 g, 0.65 mmol) is dissolved in glacial acetic acid (6 ml). Na2CO3 (0.075 g, 0.72 mmol) is added. After evolution of gas has finished, a solution of bromine (0.025 ml, 0.49 mmol) in acetic acid (3 ml) is added dropwise. Na2CO3 (0.075 g, 0.72 mmol) is added, followed by a second solution of bromine (0.025 ml, 0.49 mmol) in acetic acid (3 ml). The resulting yellow suspension is left to stir for 2 hour. The reaction is quenched by pouring onto ice water (150 ml), and neutralised using NaHCO3. The product is extracted with EtOAc and dried (MgSO4). Concentration in vacuo affords an oil, which is trituatuted with methanol to yield the title compound [M+H]+ 277.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846687B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-293e709cf8fa47f2bbb48395713b7f61 |
| Source note | uspto-grants-2014_09 |