HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → Clonazepam
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Potassium Nitrate | HCID 24434 | — |
| Edukt | 1,3-Dihydro-5-(2-chlorophenyl)-2H-1,4-benzodiozepin-2-one | HCID 14590446 | — |
| Produkt | Clonazepam | HCID 2802 | — |
Reaktionsschritte
To a solution of 13.5 g. of 5-(2-chlorophenyl)-3H-1,4-benzodiazepin-2(1H)-one in 60 ml. of concentrated sulfuric acid, a solution of 5.5 g. of potassium nitrate in 20 ml. concentrated sulfuric acid is added dropwise. The solution is then heated in a bath at 45-50° for 2 1/2 hours, cooled and poured on ice. After neutralizing with ammonia, the formed precipitate is filtered off and boiled with ethanol. A small amount of white insoluble material is then filtered off. The alcoholic solution on concentration yields crystals of 7-nitro-5-(2-chlorophenyl)-3H-1,4-benzodiazepin-2(1H)-one (clonazepam) which, after recrystallization from dichloromethane, melt at 238-240°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05706829 |
| Quelldatensatz | uspto-grants-1998_01 |
| ORD ID | ord-ad0e7fb22a6a4b19a2c390a6a34d0ab0 |
| Quellennotiz | uspto-grants-1998_01 |