HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus sulfide (P2S5) → 8-Chloro-2-(2-chloroethyl)-2,3-dihydro-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 | 8-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one | HCID 13726294 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 8-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione | HCID 13726299 | 73,2% |
Reaktionsschritte
To a solution of 43 g (0.16 mole) of 8-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in 400 ml of dry toluene was added a mixture of 23 g (0.12 mole) of phosphorus pentasulfide and 23 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux for 24 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure to give 25.5 g (55%) of orange oil which solidified on standing at room temperature. The solid was recrystallized from ethanol, m.p. 105°-106° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04727152 |
| Quelldatensatz | uspto-grants-1988_02 |
| ORD ID | ord-88fc48739333487995ac8ade2e3f01a2 |
| Quellennotiz | uspto-grants-1988_02 |