HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
6-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine → 6-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 6-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine | HCID 10198105 | — |
| Edukt | Sodium periodate | HCID 23667635 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 6-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide | HCID 10198283 | — |
Reaktionsschritte
A solution of sodium periodate (3.09 g) in water (25 ml) was added dropwise with cooling to a stirred solution of 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine (2.88 g, prepared in a similar manner to that described in the preceding paragraph) in dichloromethane (75 ml). The stirring was continued at room temperature for 19 hours. Solvent was removed from the mixture by evaporation at reduced pressure. Purification of the residue by flash chromatography using dichloromethane/ethanol (95:5) as eluent gave 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide, which was recrystallised from ethyl acetate. Yield 2.15 g (m.p. 125°-126° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05580866 |
| Quelldatensatz | uspto-grants-1996_12 |
| ORD ID | ord-e461df2775b74cb6841dc801026e2459 |
| Quellennotiz | uspto-grants-1996_12 |