HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 6-Chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Methanesulfinyl chloride | HCID 548463 | — |
| Edukt | HCID 10198105 | HCID 10198105 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 6-Chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine | HCID 9881666 | — |
Reaktionsschritte
A solution of methanesulphinyl chloride (0.98 g) in dichloromethane (10 ml) was added dropwise at room temperature to a stirred solution of 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine (1.99 g, prepared in a similar manner to its hydrochloride, Example 1 above) and triethylamine (1.01 g) in dichloromethane (50 ml). The reaction mixture was stirred at room temperature for one hour, washed with water, dried and the solvent was removed by evaporation. Purification of the residue by flash chromatography using dichloromethane/ethanol (98:2) as eluent gave 6-chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from ethylacetate/hexane. Yield 2.1 g (m.p. 82°-84° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05580866 |
| Quelldatensatz | uspto-grants-1996_12 |
| ORD ID | ord-a4b39ac55d1746fba3b43ffd23dfb566 |
| Quellennotiz | uspto-grants-1996_12 |