HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Propionyl bromide → 5-n-Butyl-4-[[2'-(N-t-butylsulfamoyl)-3-fluorobiphenyl-4-yl]methyl]-2-[2-chloro-5-(propionylamino)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Propionyl bromide | HCID 69018 | — |
| Edukt | 2(5-amino-2-chlorophenyl)-5-n-butyl-4-[[2'-(N-t-butylsulfamoyl)-3-fluorobiphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 10257760 | — |
| Katalysator | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Produkt | 5-n-Butyl-4-[[2'-(N-t-butylsulfamoyl)-3-fluorobiphenyl-4-yl]methyl]-2-[2-chloro-5-(propionylamino)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 10439146 | 84% |
Reaktionsschritte
Propionyl bromide was reacted with 2(5-amino-2-chlorophenyl)-5-n-butyl-4-[[2'-(N-t-butylsulfamoyl)-3-fluorobiphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (from Step C) in the presence of DMAP according to the procedure of Example 69. Flash chromatography of the crude product on silica gel (gradient elution with 3:1 to 1:1 hexane-EtOAc) gave an 84% yield of the title compound as a white solid, mp 103°-105° C.; homogeneous by TLC (1:1 hexane-EtOAc); mass spectrum (FAB) m/e 648 (M+Li)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05411980 |
| Quelldatensatz | uspto-grants-1995_05 |
| ORD ID | ord-fbf413da9d3c4edcb5e7e91cd01def6c |
| Quellennotiz | uspto-grants-1995_05 |