HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 4-Chloro-2-fluoro-5-propargylthioaniline
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 3-Chloro-1-propyne | HCID 12221 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Benzenethiol, 5-amino-2-chloro-4-fluoro- | HCID 11019406 | — |
| Katalysator | Benzyltributylammonium chloride | HCID 159952 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | 4-Chloro-2-fluoro-5-propargylthioaniline | HCID 13488953 | 31,9% |
Reaktionsschritte
To a mixture of 5-amino-2-chloro-4-fluorothiophenol (8.4 g), sodium hydroxide (3 g), water (80 ml), diethyl ether (40 ml) and tributylbenzylammonium chloride (0.1 g), propargyl chloride (5.2 g) was dropwise added at room temperature (ca. 20° to 25° C.), and the resultant mixture was stirred at the same temperature for 3 hours. The water layer was separated and extracted with ether. The ether extract was combined with the ether layer, washed with water, dried and concentrated under reduced pressure. The residue was crystallized from methanol to give 3.25 g of 4-chloro-2-fluoro-5-propargylthioaniline. M.P., 58°-59.5° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04752325 |
| Quelldatensatz | uspto-grants-1988_06 |
| ORD ID | ord-2c33be2925fe41ca9099c2546e231f2c |
| Quellennotiz | uspto-grants-1988_06 |