HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethyl Sulfate → N-methyl-4-(2-methyl-4-nitrophenoxy)-2-nitrobenzenamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethyl Sulfate | HCID 6497 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Bis(tetrabutylammonium) sulphate | HCID 11433187 | — |
| Edukt | 4-(2-Methyl-4-nitrophenoxy)-2-nitrobenzenamine | HCID 86650895 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | N-methyl-4-(2-methyl-4-nitrophenoxy)-2-nitrobenzenamine | HCID 86650896 | 91% |
Reaktionsschritte
To a solution of sodium hydroxide (10.2 g in 10.5 mL water) was added toluene (15 mL), 4-(2-methyl-4-nitrophenoxy)-2-nitrobenzenamine (2.00 g, 6.92 mmol), dimethyl sulfate (750 μL, 7.88 mmol) and tetrabutylammonium sulfate (0.277 g, 0.816 mmol). After stirring at room temperature, the cooled (0° C.) reaction mixture was diluted with water (100 mL) and extracted with dichloromethane (100 mL). The organic layer was washed with water and brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was chromatographed (dichloromethane) to provide the product (1.90 g, 91%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08648087B2 |
| Quelldatensatz | uspto-grants-2014_02 |
| ORD ID | ord-84b6540a481e4829af7f3db48c89bdc2 |
| Quellennotiz | uspto-grants-2014_02 |