HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
N-bromobutanimide → 5-Amino-4-bromo-6-fluoro-3-methyl-1,2-benzisothiazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | N-bromobutanimide | HCID 67184 | — |
| Edukt | 5-Amino-6-fluoro-3-methyl-1,2-benzisothiazole | HCID 12056832 | — |
| Katalysator | 1,1'-Azobis(cyclohexanecarbonitrile) | HCID 74978 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Produkt | 5-Amino-4-bromo-6-fluoro-3-methyl-1,2-benzisothiazole | HCID 18314499 | 101,3% |
Reaktionsbedingungen
| Temperatur | 70 °C |
|---|
Reaktionsschritte
To a solution of 5-amino-6-fluoro-3-methyl-1,2-benzisothiazole (0.600 g, 0.00329 mol) in 1,2-dichloroethane is added N-bromosuccinimide (0.586 g, 0.00329 mol) followed by 1,1'-azobis(cyclohexanecarbonitrile) (0.0200 g). The mixture is stirred two hours at 70° C., additional N-bromosuccinimide (0.240 g, 0.00135 mol) is added, and the mixture is stirred 40 minutes at 70° C. The mixture is then cooled to room temperature, filtered and concentrated in vacuo to obtain a residue. The residue is chromatographed on silica gel to give the title compound (0.870 g, 100%) which is identified by NMR spectral analysis.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06156700 |
| Quelldatensatz | uspto-grants-2000_12 |
| ORD ID | ord-92c8836c15f7461ba4ecbf91aba698bf |
| Quellennotiz | uspto-grants-2000_12 |