HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 3-Oxo-3-[N'-(3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-carbonyl)-hydrazino]-propionic acid tert-butyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Hydrazine | HCID 9321 | — |
| Edukt | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Edukt | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Edukt | Tert-butyl malonate | HCID 21883978 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 3-Oxo-3-[N'-(3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-carbonyl)-hydrazino]-propionic acid tert-butyl ester | HCID 23544072 | — |
Reaktionsschritte
A mixture of the hydrazine from preparation 35 (2.2 g, 10 mmol), tert-butyl malonate (1.6 g, 10 mmol), 1-hydroxybenzotriazole hydrate (2.02 g, 15 mmol), triethylamine (4.8 ml, 20 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.4 g, 12.5 mmol) in dichloromethane (50 ml) was stirred at room temperature for 5 hours. The reaction was diluted with dichloromethane (200 ml), washed with water (150 ml), dried (MgSO4) and evaporated under reduced pressure. The residual oil was purified by column chromatography on silica gel using ethyl acetate as eluant to afford the title compound, as a white solid, 1.4 g.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07084145B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-2ff387fd184f4f2e8c6f2f73124e8925 |
| Quellennotiz | uspto-grants-2006_08 |