HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Bromotrichloromethane → 3,5-Diacetoxybromobenzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Bromotrichloromethane | HCID 6383 | — |
| Edukt | Azobisisobutyronitrile | HCID 6547 | — |
| Edukt | (3-Acetyloxy-5-carbonochloridoylphenyl) acetate | HCID 11368883 | — |
| Edukt | HCID 178526253 | HCID 178526253 | — |
| Produkt | 3,5-Diacetoxybromobenzene | HCID 68648240 | 58% |
Reaktionsschritte
2.6 g (17.5 mmol) 2-mercaptopyridine-1-oxid was dissolved in 30.0 ml bromotrichloromethane and heated to reflux. A mixture of 4.04 g (15 mmol) 3,5-diacetoxybenzoylchloride and 433 mg (2.5 mmol) 2,2′-azobisisobutyronitril dissolved in 30.0 ml bromotrichlioromethane were added dropwise at the same temperature. After additional 2 hours of refluxing the reaction mixture was cooled to room temperature and concentrated in vacuum. Chromatographic purification over silica gel employing a 9:1 (v/v) mixture of n-hexane and ethyl acetate as eluting agent yielded 2.4 g of 3,5-diacetoxybromobenzene (8.7 mmol, 58%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07820848B2 |
| Quelldatensatz | uspto-grants-2010_10 |
| ORD ID | ord-4ab4561fae984b73a6af7f7733b9416b |
| Quellennotiz | uspto-grants-2010_10 |