HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 4-bromo-N-[3,5-dimethyl-4-[(nitromethyl)sulphonyl]phenyl]benzenesulphonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | p-Bromobenzenesulfonyl chloride | HCID 7396 | — |
| Edukt | Calcium Carbonate | HCID 10112 | — |
| Edukt | Ici 222155 | HCID 195716 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 4-bromo-N-[3,5-dimethyl-4-[(nitromethyl)sulphonyl]phenyl]benzenesulphonamide | HCID 18676540 | 24,2% |
Reaktionsschritte
2.0 g (20.0 mmol) of calcium carbonate and 3.8 g (14.9 mmol) of 4-bromobenzenesulphonyl chloride are successively added to a mixture of 2.4 g (9.83 mmol) of 3,5-dimethyl-4-[(nitromethyl)sulphonyl]aniline in 45 ml of anhydrous tetrahydrofuran. The reaction medium is stirred for 20 h at room temperature and is then refluxed for 48 h. After cooling, it is poured into 400 ml of water and extracted with methylene chloride. The combined organic extracts are dried over sodium sulphate and concentrated to dryness under reduced pressure. The oily residue obtained is purified by chromatography on a column of silica (eluent: methylene chloride) to give 1.1 g (24%) of 4-bromo-N-[3,5-dimethyl-4-[(nitromethyl)sulphonyl]phenyl]benzenesulphonamide.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06509499B1 |
| Quelldatensatz | uspto-grants-2003_01 |
| ORD ID | ord-b40e833edb224f349c1bd9d6ac3cf4fd |
| Quellennotiz | uspto-grants-2003_01 |