HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 3-(2-(4-(2-Methylbenzoyl)-3-chlorophenylamino)phenyl)-1,1-dimethylurea
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 4-(2-Aminophenylamino)-2-chloro-2'-methylbenzophenone | HCID 9819157 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 3-(2-(4-(2-Methylbenzoyl)-3-chlorophenylamino)phenyl)-1,1-dimethylurea | HCID 18358230 | — |
Reaktionsschritte
A mixture of 4-(2-aminophenylamino)-2-chloro-2′-methylbenzophenone (Compound 156, 1.2 g, 3.5 mmol), dimethylcarbamyl chloride (0.32 ml, 3.5 mmol) and potassium carbonate (1.0 g, 7 mmol) in N,N-dimethylformamide (20 ml) was stirred at room temperature for 16 hours. The reaction mixture was poured into water (100 ml) and was extracted with ethyl acetate (3×75 ml). The organic phase was dried (MgSO4), filtered and evaporated in vacuo to give the crude product. The crude product was purified by flash chromatography by using ethyl acetate/pentane mixtures from 1:9 to 1:1. Trituration with diethyl ether/pentane 1:1 afforded the pure title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06313174B1 |
| Quelldatensatz | uspto-grants-2001_11 |
| ORD ID | ord-0855c01a97c84672bc59d2dbeca8681d |
| Quellennotiz | uspto-grants-2001_11 |