HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus sulfide (P2S5) → 2-(2-Chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepine-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-methylnaphth[2,1-f][1,4]oxazepin-5(4H)-one | HCID 13726370 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 2-(2-Chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepine-5(4H)-thione | HCID 13726371 | 84,1% |
Reaktionsschritte
A mixture of 9.55 g of phosphorus pentasulfide and 9.5 g of potassium sulfide were ground together and added to a solution of 20.2 g (0.07 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepin-5(4H)-one in 200 ml of dry toluene. The mixture was stirred and heated at reflux for 7 hr. The hot reaction mixture was filtered and the product crystallized from the cooled filtrate. Recrystallization from chloroform gave 18 g (84%) of yellow crystals, m.p. 167°-170° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04727152 |
| Quelldatensatz | uspto-grants-1988_02 |
| ORD ID | ord-dbc1d0fc06cc4d08ac04f8d8f4685b9b |
| Quellennotiz | uspto-grants-1988_02 |