HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68432296, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Pyridine-4-carbonyl chloride | HCID 417436 | — |
| Reactant | HCID 68431688 | HCID 68431688 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68432296 | HCID 68432296 | 52.8% |
Reaction Steps
2-(2-Aminoethyl)-4-bromo-5-{[(1R,2R,3R,5S)-2,6,6-trimethylbicyclo[3.1.1]hept-3-yl]amino}pyridazin-3(2H)-one (28 mg, 0.0758 mmol) and triethylamine (21 μL, 0.152 mmol) in dichloromethane (1 mL) were stirred with pyridine-4-carbonyl chloride (20 mg, 0.112 mmol) at room temperature for 5 hours. After completion of the reaction, the reaction solution was mixed with water and extracted with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate/methanol=9/1) to give the desired product (19 mg, 52% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08440666B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-6045b6c0c2094cbfbe593ee05a88b386 |
| Source note | uspto-grants-2013_05 |