HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lithium Hydroxide → 3-Amino-4-phenoxy-5-sulfamoylbenzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lithium Hydroxide | HCID 3939 | — |
| Edukt | 3-(Aminosulfonyl)-5-nitro-4-phenoxybenzoic acid | HCID 119926 | — |
| Edukt | HCID 178418361 | HCID 178418361 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3-Amino-4-phenoxy-5-sulfamoylbenzoic acid | HCID 119927 | — |
Reaktionsschritte
A suspension of 3-nitro-4-phenoxy-5-sulphamyl-benzoic acid (20 g) in water (100 ml) was adjusted to a pH of 8 by the addition of 1N lithium hydroxide. The resulting solution was hydrogenated at room temperature and 1.1 atmosphere hydrogen pressure, using a palladium-on-carbon catalyst (0.6 g catalyst containing 10% pd). After the hydrogen uptake had become negligible, the catalyst was removed by filtration, and the 3-amino- 4-phenoxy-5-sulphamyl-benzoic acid was precipitated from the filtrate by the addition of 4N hydrochloric acid until the pH was 2.5. After recrystallization from aqueous ethanol and drying, the melting point was 255°-256°C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US03971819 |
| Quelldatensatz | uspto-grants-1976_07 |
| ORD ID | ord-6e8efe1a28ff414796e2748bc3b877ca |
| Quellennotiz | uspto-grants-1976_07 |