HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HCID 178452121, Verbindung → HCID 178452119, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | HCID 178452121 | HCID 178452121 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Lösungsmittel | N,N-dimethylformamide ethanol | HCID 19794673 | — |
| Produkt | HCID 178452119 | HCID 178452119 | 73,8% |
Reaktionsschritte
4-[(4-Nitro-1H-pyrazole-3-carbonyl)-amino]-piperidine-1-carboxylic acid tert-butyl ester (13.05 g) was dissolved in ethanol/DMF (300 ml/75 ml), treated with 10% palladium on carbon (500 mg) then hydrogenated at room temperature and pressure overnight. The catalyst was removed by filtration through Celite and the filtrate evaporated and re-evaporated with toluene. The crude material was purified by flash column chromatography eluting with EtOAc then 2% MeOH/EtOAc then 5% MeOH/EtOAc. Product containing fractions were combined and evaporated to give 8.78 g of 4-[(4-amino-1H-pyrazole-3-carbonyl)-amino]-piperidine-1-carboxylic acid tert-butyl ester as a brown foam. (LC/MS: Rt 1.91, [M+H]+ 310).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07745638B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-6ce96a5154a4438bac2f558f0b1ed6a2 |
| Quellennotiz | uspto-grants-2010_06 |