HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → n-{3-Nitro-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | 3,5-Bis(trifluoromethyl)benzylamine | HCID 521099 | — |
| Reactant | N-(4-fluoro-3-nitrophenyl)benzenesulfonamide | HCID 4599069 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | n-{3-Nitro-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide | HCID 22621842 | — |
Reaction Steps
N-{4-fluoro-3-nitro-phenyl}-benzenesulphonamide (3.0 g, 10 mmol), 3,5-bis-trifluoromethylbenzylamine (3.0 g, 12.5 mmol) and N-methylmorpholine (2.2 mL, 20 mmol) in 25 mL dimethylsulphoxide are kept for 6 h at 60-100° C., diluted with 150 mL ethyl acetate, washed with water, dilute hydrochloric acid and water again, dried and concentrated by evaporation until not quite dry. The residue is combined with 80 mL EtOH and evaporated down to a residual volume of about 50 mL. The crystals precipitated after cooling are filtered off and washed with EtOH and petroleum ether.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06365584B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-85ceb8881f0148d7b79e1914119d07d7 |
| Source note | uspto-grants-2002_04 |