HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Benzoic acid, 3-sulfo- → 3-(2-Methyl-propane-1-sulfonyl)-benzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Benzoic acid, 3-sulfo- | HCID 8477 | — |
| Edukt | Isobutyl iodide | HCID 10556 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Lösungsmittel | Dimethylacetamide | HCID 31374 | — |
| Produkt | 3-(2-Methyl-propane-1-sulfonyl)-benzoic acid | HCID 22397459 | — |
Reaktionsschritte
To a suspension of 3-sulfo-benzoic acid (1 g) and potassium carbonate (1.2 g) in dimethylacetamide (10 ml) was added iso-butyl iodide (0.65 ml). The mixture was heated by microwaves (600W) at 150° C. for 15 minutes. The reaction mixture was partitioned between water (100 ml) and ethyl acetate (100 ml), the aqueous layer was separated, acidified to pH 1 with HCl (2N) and extracted with ethyl acetate (100 ml). The extract was evaporated to leave a residue which was purified by flash chromatography (Biotage 12S eluting with ethyl acetate:hexane:acetic acid, 29:70:1) to give the title product as a white solid (0.34 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07238811B2 |
| Quelldatensatz | uspto-grants-2007_07 |
| ORD ID | ord-4320a0a205104117aa46ccbf8bd7b9e1 |
| Quellennotiz | uspto-grants-2007_07 |