HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Anhydride → 1-(5-Bromo-3-methyl-1H-indazol-1-yl)ethan-1-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Anhydride | HCID 7918 | — |
| Edukt | Isoamyl Nitrite | HCID 8053 | — |
| Edukt | 18-Crown-6 | HCID 28557 | — |
| Edukt | Potassium Acetate | HCID 517044 | — |
| Edukt | 4-Bromo-2-ethylaniline | HCID 2801283 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | 1-(5-Bromo-3-methyl-1H-indazol-1-yl)ethan-1-one | HCID 59127382 | — |
Reaktionsschritte
Acetic anhydride (4.73 ml) was added to the mixture of 4-bromo-2-ethylaniline (5.0 g) and KOAc (2.94 g) in CHCl3 (70 ml) and stirred for 30 minutes at reflux. Then isoamyl nitrite (6.65 ml) and 18-crown-6-ether (660 mg) was added to the reaction mixture and stirred for 12 h. under reflux. The reaction mixture was diluted with CHCl3, washed with water, and dried over sodium sulfate. After filtration and concentration, the residue was purified by silica gel chromatography (hexane/EtOAc), and crystallized from mixed solvent of hexane and CHCl3 to give intended compound as a yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08524730B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-7b5dffd064424629bd0d34f8d159136b |
| Quellennotiz | uspto-grants-2013_09 |