HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 69517824, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dabco | HCID 9237 | — |
| Reactant | Carbamic chloride, N-methyl-N-phenyl- | HCID 77969 | — |
| Reactant | HCID 178479717 | HCID 178479717 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69517824 | HCID 69517824 | 55% |
Reaction Steps
A solution of pyridine-2-carboxylic acid (6-hydroxy-pyridin-3-yl)-amide hydrochloride (0.50 g, 1.99 mmol), N-methyl-N-phenylcarbamoyl chloride (0.44 g, 2.59 mmol) and 1,4-diazabicyclo[2,2,2]octane (0.54 g, 4.81 mmol) in dimethylformamide (15 mL) was stirred at room temperature for 1 hour. Water was added and the solids were isolated by suction, redissolved in dichloromethane. The solution was dried over sodium sulphate, filtered and evaporated in vacuo. The residue was purified by flash column chromatography (SiO2, ethyl acetate:heptane 50:50) yielding the title compound (0.38 g, 55% yield) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07279470B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-3159df573e324f3c846f2c04fbefc166 |
| Source note | uspto-grants-2007_10 |