HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus sulfide (P2S5) → 2-(2-Chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepine-5(4H)-thione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Edukt | Potassium Sulfide | HCID 162263 | — |
| Edukt | 2-(2-Chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepin-5(4H)-one | HCID 13726297 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | 2-(2-Chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepine-5(4H)-thione | HCID 13726302 | 86,3% |
Reaktionsschritte
To a solution of 10.3 g (0.04 mole) of 2-(2-chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepin-5(4H)-one in 200 ml of chloroform was added a mixture of 5.7 g (0.03 mole) of phosphorus pentasulfide and 5.7 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux under nitrogen atmosphere for 5 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure. The residue, an orange solid, was recrystallized from ethanol to give 7.4 g (65%) of product, m.p. 98°-100° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04727152 |
| Quelldatensatz | uspto-grants-1988_02 |
| ORD ID | ord-ffbaf1c2ea5949e094d1b0c62e55de55 |
| Quellennotiz | uspto-grants-1988_02 |