HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Thiosulfate → 6-Chloro-3-iodo-2-phenylimidazo[1,2-b]pyridazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Iodine chloride | HCID 24640 | — |
| Reactant | Imidazo(1,2-b)pyridazine, 6-chloro-2-phenyl- | HCID 137233 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 6-Chloro-3-iodo-2-phenylimidazo[1,2-b]pyridazine | HCID 24862471 | 92.9% |
Reaction Steps
To a solution, cooled to 0° C., of 10.4 g (45.4 mmol) of 6-chloro-2-phenylimidazo[1,2-b]pyridazine (CAS No.: 1844-53-7) in 500 mL of chloroform is rapidly added dropwise a solution of 11.1 g (68.1 mmol) of iodine monochloride in 100 mL of chloroform. After cooling to room temperature and stirring for 1 hour, the mixture is treated with aqueous 5% sodium thiosulfate solution. The product is extracted with dichloromethane and the organic phase is dried over sodium sulfate and concentrated under reduced pressure. The residue is triturated in 150 ml of acetonitrile containing a few mL of isopropyl alcohol and the solid is isolated after filtration. 15 g of a yellow powder are isolated after drying under vacuum.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08354405B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-501a285d2d334149a20bdc920b7ba632 |
| Source note | uspto-grants-2013_01 |