Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Hydrogen Sulfide | HCID 402 | — |
| Reactant | HCID 18989286 | HCID 18989286 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 53784070 | HCID 53784070 | — |
Reaction Steps
4.6 g (7.78 mmol) of 3-(6,7-dimethoxynaphthalene-2-sulfonylamino)-1-[2-(4-cyanophenyl)-1-piperidinocarbonylethyl]-2-pyrrolidinone were dissolved in 5 ml of triethylamine and 80 ml of pyridine, and hydrogen sulfide was passed into saturation. The mixture was left to stand overnight and subsequently added dropwise to a mixture of 600 g of ice and 100 ml of concentrated hydrochloric acid. The precipitate was filtered off with suction and dissolved in THF, and the solution was dried over magnesium sulfate and concentrated. The residue was mixed with ether and, after stirring at room temperature for 30 min, the precipitate was filtered off with suction. The slightly impure 3-(6,7-dimethoxynaphthalene-2-sulfonylamino)-1-[2-(4-aminothiocarbonylphenyl)-1-piperidinocarbonylethyl]-2-pyrrolidinone was used without further purification in the next stage.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05489583 |
|---|
| Source dataset | uspto-grants-1996_02 |
|---|
| ORD ID | ord-197403a17feb428ca82fb715606563ac |
|---|
| Source note | uspto-grants-1996_02 |
|---|