HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus sulfide (P2S5) → HCID 22041438, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | HCID 22041454 | HCID 22041454 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22041438 | HCID 22041438 | 77% |
Reaction Steps
Into 5 mL of 1,4-dioxane solution of 150 mg of 4-(5-fluoro-3-methylbenzo[b]thiophene-2-yl)sulfonamido-3-methanesulfonyl-N-(2-oxopropyl)benzamide was added 135 mg of diphosphorus pentasulfide, followed by 4.5 hours of heating under refluxing. The reaction was terminated by adding water to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, successively and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure and the resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=2/1 to 1/1) to obtain 115 mg of the title compound as amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07399781B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-d367250ffad44e4d9d302c20bad8c185 |
| Source note | uspto-grants-2008_07 |