HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 53870579, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 6-[3-(2-Chloromethyl-3-methylpyridin-4-ylsulfanyl)propylsulfanyl]-3-nitroimidazo[1,2-b]pyridazine | HCID 18799383 | — |
| Reactant | 2-Mercapto-4-methylpyrimidine hydrochloride | HCID 178428687 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 53870579 | HCID 53870579 | — |
Reaction Steps
A suspension of 4-methyl-pyrimidine-2-thiol hydrochloride (0.46 g, 2.8 mmol) and 6-[3-(2-chloromethyl-3-methyl-pyridin-4-ylsulfanyl)-propylsulfanyl]-3-nitroimidazo[1,2-b]pyridazine (1.03 g, 2.5 mmol) in 2-propanol (50 ml) is heated under reflux for 4 h under a nitrogen atmosphere. After cooling, the mixture is treated with ice water (100 ml), adjusted to pH 10 with 40% strength sodium hydroxide solution, and extracted with ethyl acetate. The combined extracts are washed with sodium carbonate solution, dried over magnesium sulfate and evaporated in vacuo. The residue is chromatographed (silica, toluene/dioxane 2:1) and crystallized from acetonitrile to give the title compound as a colourless solid, 0.49 g (39%). M.p. 136-8° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06043242 |
| Source dataset | uspto-grants-2000_03 |
| ORD ID | ord-b75ef14d22d84e5fb97083b1883e6b0a |
| Source note | uspto-grants-2000_03 |