HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-Chlorobenzoic Acid → HCID 10010234, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-Chlorobenzoic Acid | HCID 8374 | — |
| Edukt | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Edukt | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Edukt | 5-n-butyl-2,4-dihydro-2-[5-(propionylamino)-2-(trifluoromethyl)phenyl]-4-[(2'-sulfamoylbiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one | HCID 10258037 | — |
| Produkt | HCID 10010234 | HCID 10010234 | 50% |
Reaktionsschritte
Following the procedure of Example 51, 5-n-butyl-2,4-dihydro-2-[5-(propionylamino)-2-(trifluoromethyl)phenyl]-4-[(2'-sulfamoylbiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one (from Step F) was reacted with 2-chlorobenzoic acid (3 equivalents), CDI (3 equiv), and DBU (3 equiv). Flash chromatography of the crude product on silica gel (gradient elution with 0.5-2% MeOH in CH2Cl2) afforded a 50% yield of the title compound as a solid, mp 102°-105° C.; homogeneous by TLC in 9:1 CH2Cl2 --MeOH; mass spectrum (FAB) m/e 740 (M+1)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05411980 |
| Quelldatensatz | uspto-grants-1995_05 |
| ORD ID | ord-1df9d20720c94b3b98ac3118edd9fafa |
| Quellennotiz | uspto-grants-1995_05 |