HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 18919022, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-(4-Chlorobenzoyl)benzyl bromide | HCID 9839651 | — |
| Reactant | HCID 18918833 | HCID 18918833 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18919022 | HCID 18919022 | 59.7% |
Reaction Steps
In DMF (5 ml) was dissolved 6-methyl-1,2,3,4-tetrahydropyrido[2,3-d]pyridazin-5(6H)-one (116 mg) followed by addition of sodium hydride (60%) (56 mg), and the mixture was stirred at room temperature for 30 minutes. Then, 4-(4-chlorobenzoyl)benzyl bromide (341 mg) was added and the mixture was further stirred at room temperature for 1 hour. This reaction mixture was diluted with water and extracted with ethyl acetate-THF. The organic layer was serially washed with water and saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel chromatography (ethyl acetate) to provide 165 mg of the title compound as yellow amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05753664 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-650c04555ce945c7a5a12d5cc75b5a2e |
| Source note | uspto-grants-1998_05 |