HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Nitrate → 10-Methyl-7-nitro-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H,11aH)-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Nitrate | HCID 24434 | — |
| Edukt | 10-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H,11aH)-dione | HCID 9859436 | — |
| Lösungsmittel | Sulfuric Acid | HCID 1118 | — |
| Produkt | 10-Methyl-7-nitro-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H,11aH)-dione | HCID 70133774 | — |
Reaktionsschritte
To 10-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H,11aH)-dione (5.7 g, 24.7 mmol) in concentrated sulfuric acid (60 ml) at 0° C. was added potassium nitrate (2.62 g, 25.9 mmol). After stirring for 2 h the mixture was dumped onto ice (500 g) and extracted with ethyl acetate (5×75 ml). The combined extracts were washed with water, dried over magnesium sulfate, filtered, and concentrated to a solid which was recrystallized from ethyl acetate-hexane (5.2 g, 77%), m.p. 160-162° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06140322 |
| Quelldatensatz | uspto-grants-2000_10 |
| ORD ID | ord-8635e32687494b0d920640d321ee7743 |
| Quellennotiz | uspto-grants-2000_10 |