HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → 3,3-Difluoro-3-(4-fluorophenyl)-propane-1-thiol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | ethanethioic acid S-[3,3-difluoro-3-(4-fluorophenyl)-propyl]ester | HCID 86720161 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 3,3-Difluoro-3-(4-fluorophenyl)-propane-1-thiol | HCID 86720162 | 92,4% |
Reaktionsschritte
To a solution of ethanethioic acid S—[3,3-difluoro-3-(4-fluorophenyl)-propyl]ester (0.26 g, 1.05 mmol) in EtOH (3 ml) is added 35% aqueous sodium hydroxide (3 ml) at 0° C. and the reaction mixture is stirred at RT for 1 h. After completion of the reaction, the solvent is distilled off and the residue is diluted with water (10 ml) before acidification with 2N hydrochloric acid to pH 2. The aqueous layer is extracted with EtOAc (3×15 ml) and the combined organic layers are washed with water (20 ml), brine (20 ml), dried over anhydrous sodium sulfate and evaporated to get 3,3-difluoro-3-(4-fluorophenyl)-propane-1-thiol (0.20 g, 0.97 mmol, 92%), which is used in the next step without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09284286B2 |
| Quelldatensatz | uspto-grants-2016_03 |
| ORD ID | ord-f3e8f823b79449ababa92e55b3114782 |
| Quellennotiz | uspto-grants-2016_03 |