HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 18919155, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 18919103 | HCID 18919103 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 18919155 | HCID 18919155 | 19% |
Reaction Steps
In dioxane (15 ml) was dissolved 1-[4-(4-chlorobenzoyl)benzyl]-4,7-dichloropyrrolo [2,3-d]pyridazine (1.08 g). Then, sodium hydroxide (4.42 g) and water (5 ml) were added and the mixture was refluxed for 69 hours. This reaction mixture was diluted with water (120 ml) and the resulting crystals were collected by filtration. The crystals were purified by silica gel column chromatography (stationary phase 50 g; dichloromethane: ether=1:0-9:1; ethyl acetate: methanol=1:9) to provide 416 mg (yield 40%) of the title compound 1-[4-(4-chlorobenzoyl)benzyl]-4-chloropyrrolo [2,3-d]pyridazin-7(6H)-one(A) and 196 mg (yield 19%) of the title compound 1-[4-(4-chlorobenzoyl)benzyl]-7-chloropyrrolo [2,3-d]pyridazin-4(5H)-one(B).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05753664 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-012056deda354e83b908bcb59a5b38e9 |
| Source note | uspto-grants-1998_05 |