HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → methyl 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Propanal, 3-ethoxy- | HCID 17755 | — |
| Edukt | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Edukt | HCID 22328936 | HCID 22328936 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Produkt | methyl 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate | HCID 22329178 | 96,9% |
Reaktionsschritte
To a solution of methyl 7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (400 mg) and 3-ethoxypropionaldehyde (0.53 g) in 1,2-dichloroethane (10 ml) was added sodium triacetoxyborohydride (0.66 g) at room temperature, and the mixture was stirred for 20 hours. To the reaction system was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with magnesium sulfate. After concentration under reduced pressure, the residue was separated and purified with column chromatography (ethyl acetate:hexane=1:4→1:3) to give methyl 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (475 mg) as yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06936602B1 |
| Quelldatensatz | uspto-grants-2005_08 |
| ORD ID | ord-a022a797e2b34410ba85a15592ad2b8e |
| Quellennotiz | uspto-grants-2005_08 |