HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl 2-bromo-3-nitrobenzoate → 9-Nitro-1,2,3,4-tetrahydro-5H-1,4-benzodiazepin-5-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl 2-bromo-3-nitrobenzoate | HCID 79263 | — |
| Edukt | Ethylenediamine monohydrate | HCID 12200817 | — |
| Lösungsmittel | 1-Butanol | HCID 263 | — |
| Produkt | 9-Nitro-1,2,3,4-tetrahydro-5H-1,4-benzodiazepin-5-one | HCID 2771611 | — |
Reaktionsschritte
A mixture of 11.7 parts of methyl 2-bromo-3-nitrobenzoate, 8.1 parts of 1,2-ethanediamine monohydrate and 40 parts of 1-butanol was stirred for 1/2 at reflux temperature. The reaction mixture was evaporated and the residue was diluted with 50 parts of water. The precipitate was filtered off and washed with water and 2-propanol. It was then recrystallized from 2-methoxyethanol, yielding 6.5 parts of 2,3,4,5-tetrahydro-9-nitro-1H-1,4-benzodiazepin-5-one; mp. 191°-195° C. (interm. 1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05371079 |
| Quelldatensatz | uspto-grants-1994_12 |
| ORD ID | ord-b5bb6de2332b49a1ae470df8ba774161 |
| Quellennotiz | uspto-grants-1994_12 |