HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 59136020, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | N-[(1-benzyl-4-hydroxypiperidin-4-yl)methyl]-7-[methyl(2-thienylsulfonyl)amino]-1H-indole-2-carboxamide | HCID 59136004 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59136020 | HCID 59136020 | 5% |
Reaction Steps
To a solution of N-[(1-benzyl-4-hydroxypiperidin-4-yl)methyl]-7-[methyl(2-thienylsulfonyl)amino]-1H-indole-2-carboxamide (1.30 g) in a mixed solvent of toluene (60 ml) and tetrahydrofuran (30 ml) was added Lawesson's reagent (1.94 g), and the mixture was heated under reflux for 3 hr. The reaction solution was concentrated under reduced pressure, and the residue was purified by basic silica gel column chromatography (ethyl acetate:hexane=5:95-40:60), and recrystallized from ethyl acetate-hexane to give the title compound (0.063 g, yield 5%) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410087B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-e1327520a69d42a9bc7a5bd65b8e0dc0 |
| Source note | uspto-grants-2013_04 |