HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-Nitroimidazole → 4[(2-nitro-1H-imidazol-1-yl)methyl]-1-piperidinecarboxaldehyde
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-Nitroimidazole | HCID 10701 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | N-Formyl-4-bromomethylpiperidine | HCID 19812293 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 4[(2-nitro-1H-imidazol-1-yl)methyl]-1-piperidinecarboxaldehyde | HCID 20239747 | 25,3% |
Reaktionsschritte
The mixture of 2-nitroimidazole (4.5 g, 40 mM) and 50% by weight NaH in mineral oil (1.92 g, 41 mM) in dimethylformamide (40 ml) was stirred at room temperature for 1/2 hr. A solution of 4-bromomethyl-1-piperidinecarboxaldehyde (8.3 g, 40 mM) in dimethylformamide (10 ml) was added to the above mixture and heated at 120° C. for 1/2 hr. After the reaction, solvent was removed in vacuo and water (50 ml) was added and the mixture was extracted with ethylacetate (2×75 ml). The extracts, dried over Na2SO4 was stripped to dryness which was then purified on silica gel column, eluted with 5% volume MeOH-95% volume CH2Cl2, to give 4[(2-nitro-1H-imidazol-1-yl)methyl]-1-piperidinecarboxaldehyde (2.4 g, 10 mL) in 25% yield.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04537969 |
| Quelldatensatz | uspto-grants-1985_08 |
| ORD ID | ord-435e27e741f948dea9e2f64143d8efc5 |
| Quellennotiz | uspto-grants-1985_08 |