HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Chloroperbenzoic acid → HCID 15952963, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Chloroperbenzoic acid | HCID 70299 | — |
| Reactant | HCID 15952855 | HCID 15952855 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 15952963 | HCID 15952963 | 38% |
Reaction Steps
4-chloroperbenzoic acid (36 mg, 0.134 mmol, 1 eq) is added to a solution of 1-{[6-(methylthio)-2-(trifluoromethyl)imidazo[1,2-b]pyridazin-3-yl]methyl}-4-propyl pyrrolidin-2-one 33 (50 mg, 0.134 mmol) in chloroform (2 ml) at −30° C. After 30 minutes, the mixture is warmed to room temperature then stirred for additional 16 hours. After hydrolysis with a saturated aqueous NaHCO3 solution (2 ml) and extraction with CHCl3 (2 ml), the cumulated organic layers are dried over MgSO4 and condensed under reduced pressure. The resulting crude product is purified by reverse phase liquid chromatography (gradient acetonitrile/water/TFA) to yield 1-{[6-(methylsulfinyl)-2-(trifluoromethyl)imidazo[1,2-b]pyridazin-3-yl]methyl}-4-propylpyrrolidin-2-one 82.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08518943B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-4c3e964d604249cbb22b40ee05280752 |
| Source note | uspto-grants-2013_08 |