HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Azobisisobutyronitrile → 6-Bromo-7-(bromomethyl)-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Azobisisobutyronitrile | HCID 6547 | — |
| Edukt | N-bromobutanimide | HCID 67184 | — |
| Edukt | 6-Bromo-1,1,4,4,7-pentamethyl-1,2,3,4-tetrahydronaphthalene | HCID 10039346 | — |
| Lösungsmittel | Carbon Tetrachloride | HCID 5943 | — |
| Produkt | 6-Bromo-7-(bromomethyl)-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene | HCID 23498953 | — |
Reaktionsschritte
The mixture of 6-bromo-7-methyl-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene (4.20 g, 15 mmol), NBS (3.20 g, 18 mmol), 2,2′-azobisisobutyronitrile (0.3 g, 1.8 mmol) and CCl4 (120 mL) was heated at reflux for 16 hours. The mixture was concentrated under reduced pressure to about 50 mL. The reaction was then filtered, and the solid was washed with Et2O (20 mL). The combined organic solution was then concentrated under vacuum to generate crude product. Crude 91.2 was generated as a brown oil and used directly in the next step without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07582803B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-4d9162968f024969a493a6db5ba91605 |
| Quellennotiz | uspto-grants-2009_09 |