HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Azobisisobutyronitrile → ethyl 2-(3-bromo-5-methyl-2H-indazol-2-yl)benzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Azobisisobutyronitrile | HCID 6547 | — |
| Edukt | N-bromobutanimide | HCID 67184 | — |
| Edukt | ethyl 2-(5-methyl-2H-indazol-2-yl)benzoate | HCID 20094524 | — |
| Lösungsmittel | Carbon Tetrachloride | HCID 5943 | — |
| Produkt | ethyl 2-(3-bromo-5-methyl-2H-indazol-2-yl)benzoate | HCID 20094549 | 80,2% |
Reaktionsschritte
Carbon tetrachloride (26 ml) was added to ethyl 2-(5-methyl-2H-indazol-2-yl)benzoate (1.43 g, 5.10 mmol) as obtained in Reference Example 3 and the mixture was stirred. Thereto were added N-bromosuccinimide (0.908 g, 5.10 mmol) and azobisisobutyronitrile (78 mg, 0.48 mmol), and the mixture was refluxed under heating for 3 hours. After cooling, the mixture was filtered, and the cake was washed twice with carbon tetrachloride (5 ml). The filtrate was concentrated, and subjected to flash chromatography on silica gel using a mixed solvent of hexane/ethyl acetate (8:1-3:1), whereby 1.47 g of ethyl 2-(3-bromo-5-methyl-2H-indazol-2-yl)benzoate was obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05387684 |
| Quelldatensatz | uspto-grants-1995_02 |
| ORD ID | ord-a396e4a2660146bdb25caf16e91adfc5 |
| Quellennotiz | uspto-grants-1995_02 |