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 | — |
| 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 stirred at reflux overnight. The mixture was diluted with ethyl acetate (200 mL) and washed with aqueous NaHCO3, water, and brine and dried over Na2SO4. After filtration and concentration, the residue was dissolved in dichloromethane and loaded on a column and eluted with dichloromethane (500 mL), 5% 7N NH3 in 10% methanol in dichloromethane (1.5 L) to give the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029404B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-f0bd433cf5894caba967378264476c30 |
| Source note | uspto-grants-2015_05 |