HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Benzyl mercaptan → Benzyl(3-bromo-2-chlorophenyl)sulfane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Benzyl mercaptan | HCID 7509 | — |
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 1-Bromo-2-chloro-3-fluorobenzene | HCID 3739301 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Water ethylacetate | HCID 22728543 | — |
| Produkt | Benzyl(3-bromo-2-chlorophenyl)sulfane | HCID 66911177 | — |
Reaktionsschritte
To stirred phenyl-methanethiol (14.8 g, 119.36 mmol) in 175 ml DMF was added Cs2CO3 (38.89 g, 119.36 mmol) under argon. After 10 min. 1-bromo-2-chloro-3-fluoro-benzene (25 g, 119.36 mmol) in 25 ml DMF was added and stirring was continued overnight at RT and then 3 h at 80° C. After cooling the mixture was diluted with ethyl acetate/water and washed subsequently with 1 N HCl and brine. The organic layer was dried with MgSO4, filtered and evaporated. Purification by chromatography on silica gel yielded 22 g (59%) as an amorphous, colorless solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08835653B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-9df104e0df9f402e818fccf9e21a172f |
| Quellennotiz | uspto-grants-2014_09 |