HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon Disulfide → HCID 18918808, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon Disulfide | HCID 6348 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyldesphenylchloridazon | HCID 594330 | — |
| Reactant | 4-(4-Fluorobenzoyl)benzyl bromide | HCID 4729013 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18918808 | HCID 18918808 | 72.9% |
Reaction Steps
In DMF (10 ml) was dissolved 5-amino-4-chloro-2-methyl-3(2H)-pyridazinone (638 mg) followed by addition of 60% sodium hydride (384 mg), and the mixture was stirred at room temperature for 10 minutes. Then, carbon disulfide (365 mg) was added and the mixture was further stirred at 80° C. for 1 hour. Thereafter, 4-(4-fluorobenzoyl)benzyl bromide (1.4 g) was added and the mixture was stirred at room temperature for 1 hour. This reaction mixture was extracted with ethyl acetate-THF and the organic layer was washed serially with water and saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel chromatography (hexane: ethyl acetate =1:1) to provide 1.2 g of white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05753664 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-272a232e11fd462ebb03db7980be83c6 |
| Source note | uspto-grants-1998_05 |