HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus sulfide (P2S5) → 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 | 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one | HCID 13726293 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 2-(2-Chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione | HCID 13726298 | — |
Reaktionsschritte
A mixture of 18.5 g (0.0834 mole) of phosphorus pentasulfide and 18.5 g potassium sulfide was ground together and added to a solution of 100 g (0.417 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in dry toluene, the mixture refluxed 24 hr. and filtered. The filtrate was concentrated and partitioned between chloroform and diluted sodium hydroxide. The chloroform layer was concentrated and the residue was crystallized several times from ethanol. Yield of product was 55 g (52%), m.p. 105°-108° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04727152 |
| Quelldatensatz | uspto-grants-1988_02 |
| ORD ID | ord-8b003d3c47b34351abfb5f38c61627e5 |
| Quellennotiz | uspto-grants-1988_02 |