HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diazepam → 10-chloro-2-chloromethyl-2,3,5,11b-tetrahydro-7-methyl-11b-phenyloxazolo[3,2-d][1,4]benzodiazepin-6(7H)-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diazepam | HCID 3016 | — |
| Edukt | Epichlorohydrin | HCID 7835 | — |
| Edukt | Aluminum(III) Chloride | HCID 6451240 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Produkt | 10-chloro-2-chloromethyl-2,3,5,11b-tetrahydro-7-methyl-11b-phenyloxazolo[3,2-d][1,4]benzodiazepin-6(7H)-one | HCID 21409971 | — |
Reaktionsschritte
A mixture of 10 g. (35 mmole) of 7-chloro-1,3-dihydro-1-methyl-5-phenyl-2H-1,4-benzodiazepin-2-one, 10 g. of aluminum chloride, and 200 ml. of dried benzene was treated with 30 ml. of 1-chloro-2,3-epoxypropane in 100 ml. of benzene. The reaction mixture was stirred overnight. Work-up as in Method A, Example 5, above gave 32 g. of a crude oil. The oil was dissolved in benzene, filtered over Florisil, evaporated to dryness and crystallized from ether-petroleum ether to give the above-titled product as colorless needles, m.p. 140°-142°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04049667 |
| Quelldatensatz | uspto-grants-1977_09 |
| ORD ID | ord-9e23801453d14c52bc40181f34282f4d |
| Quellennotiz | uspto-grants-1977_09 |