HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 86028266, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 3-Bromo-2-chlorobenzoic acid | HCID 33124 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86028266 | HCID 86028266 | — |
Reaction Steps
To a solution of 3-bromo-2-chlorobenzoic acid (1.79 mmol) in 12 mL THF were added N,O-dimethylhydroxylamine HCl (2.32 mmol), EDC.HCl (4.29 mmol) and pyridine (2.68 mmol) at 0° C. The cooling bath was removed and stirring was continued at RT overnight. The reaction was diluted with DCM and extracted with water, sat. aq. NH4Cl solution, sat. aq. NaHCO3 solution, dried over MgSO4 and concentrated in vacuo. Purification by CC (KP-SIL™ from Biotage) using Hept to EtOAc gives the desired compound as colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09221832B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-567ead448a434567a383dfdc81e26b5e |
| Source note | uspto-grants-2015_12 |