HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 5,8-Dibromo-2,3-diphenylquinoxaline
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Benzil | HCID 8651 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 3,6-Dibromobenzene-1,2-diamine | HCID 11821532 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | 5,8-Dibromo-2,3-diphenylquinoxaline | HCID 22475901 | — |
Reaktionsschritte
The detailed preparation procedure is as follows: 3,6-dibromo-o-phenylene diamine (1.0 g, 3.7 mmol) was added to a solution of compound benzil (0.39 g, 1.84 mmol) in acetic acid (20 mL) at 120□, then the mixture was mixed uniformly. After refluxed for 12 hours, the fluid reactant was poured into water, and neutralized with sodium bicarbonate until neutral, then extracted with chloroform and washed with saturated brine, dried over anhydrous sodium sulfate, then it was vacuum evaporated to remove the solvent, and the resulting crude product was purified by column chromatography to give a white solid, and then it was purified by recrystallization from chloroform/n-hexane to give a white solid powder. The test result is: MS (EI) m/z: 440(M+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08853348B2 |
| Quelldatensatz | uspto-grants-2014_10 |
| ORD ID | ord-036f8be6036b4223b33192d6e1f3491f |
| Quellennotiz | uspto-grants-2014_10 |