HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 4-(1-Cyclopropylpiperidin-4-ylamino)-3-nitrobenzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1-Cyclopropylpiperidin-4-amine | HCID 16227644 | — |
| Reactant | 4-Fluoro-3-nitrobenzenesulfonamide | HCID 16782487 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | 4-(1-Cyclopropylpiperidin-4-ylamino)-3-nitrobenzenesulfonamide | HCID 26042751 | — |
Reaction Steps
To a solution of 4-fluoro-3-nitrobenzenesulfonamide (1.26 g) and 1-cyclopropylpiperidin-4-amine (0.802 g) in tetrahydrofuran (20 mL) was added N,N-diisopropylethylamine (2.22 g) and 4-dimethylaminopyridine (35 mg). The mixture was heated at reflux for 18 hours and upon cooling was diluted with ethyl acetate (200 mL) and aqueous NaHCO3. The crude product was isolated by concentration of the organic layer and was purified on silica gel, which was eluted with 5% methanolic ammonia in methylene chloride to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045420B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-61c715b59c8f414a9d15c6a17c95587f |
| Source note | uspto-grants-2015_06 |