HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → 3-[4-(3-Cyano-phenyl)-piperazin-1-ylmethyl]-benzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 3-[4-(3-Cyano-phenyl)-piperazin-1-ylmethyl]-benzoic acid methyl ester | HCID 67508190 | — |
| Lösungsmittel | MeOH tetrahydrofuran | HCID 21899815 | — |
| Produkt | 3-[4-(3-Cyano-phenyl)-piperazin-1-ylmethyl]-benzoic acid | HCID 67507474 | — |
Reaktionsschritte
Dissolve 3-[4-(3-cyano-phenyl)-piperazin-1-ylmethyl]-benzoic acid methyl ester into 10 mL of 1:1 THF/MeOH and add 2 mL of 15% NaOH. Stir the mixture overnight and concentrate to dryness. Dissolve the residue in 5% HCl and apply to Dowex column. Rinse the resin with 2×20 mL H2O, 2×20 mL MeOH and 2×20 mL of dichloromethane. Liberate the basic residues by washing the resin with 3×20 mL of 10% NH3/MeOH to give 0.26 g 3-[4-(3-cyano-phenyl)-piperazin-1-ylmethyl]-benzoic acid as a white solid. 1H NMR indicates some contamination with starting amine. The crude intermediate is carried on without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09000154B2 |
| Quelldatensatz | uspto-grants-2015_04 |
| ORD ID | ord-99acd1a56d654399a9a9ef07954e96d2 |
| Quellennotiz | uspto-grants-2015_04 |