HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 8-Hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium metaborate | HCID 145326 | — |
| Edukt | 8-formyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine | HCID 10893077 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 8-Hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine | HCID 18183191 | 78,4% |
Reaktionsbedingungen
| Temperatur | 20 °C |
|---|
Reaktionsschritte
2.5 g (7.41 mmol) of 8-formyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine (I, stage A) is suspended in THF:water=1:1 and mixed with 0.14 g (3.7 mmol) of sodium boranate while being stirred and cooled to 20° C. After 45 minutes of stirring, it is filtered and the crude product is precipitated from the filtrate with 130 ml of water. 2.35 g, which is recrystallized from a mixture of 6.3 ml of dimethylformamide and 1.3 ml of water, is obtained. 1.97 g (78%) of the title compound with a melting point of 175° C. (decomposition) is obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06600036B2 |
| Quelldatensatz | uspto-grants-2003_07 |
| ORD ID | ord-53cc19ebc4ab4e9983c0880dc0bc2169 |
| Quellennotiz | uspto-grants-2003_07 |