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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 69056Erstellt: 24. Oktober 2026

Potassium Carbonate → 1-Ethyl-3,3,5-trimethyl-7-[3-(2-phenyl-benzoimidazol-1-yl)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione hydrochloride

https://huagongshe.com/de/reaction/69056

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktPotassium CarbonateHCID 11430—
Edukt2-PhenylbenzimidazoleHCID 12855—
EduktEthanol hydrochlorideHCID 21887872—
Edukt1-Ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dioneHCID 68672792—
LösungsmittelIsopropanolHCID 3776—
LösungsmittelDimethylformamideHCID 6228—
Produkt1-Ethyl-3,3,5-trimethyl-7-[3-(2-phenyl-benzoimidazol-1-yl)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione hydrochlorideHCID 70656674—

Reaktionsbedingungen

Temperatur60 °C

Reaktionsschritte

2-Phenyl-1H-benzimidazole (0.2 g) and potassium carbonate (0.29 g) were added to a DMF solution (5 ml) of 1-ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.49 g). The mixture was stirred at 60° C. for 7 hours. The reaction mixture was poured to ice water (50 ml), and the generated insoluble matter was separated. The insoluble matter was dissolved in ethyl acetate. The liquid was dried over sodium sulfate and condensed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:3). The purified product was condensed under reduced pressure. A 1N-hydrogen chloride ethanol solution (1.0 ml) was added to an isopropyl alcohol solution of the residue. The mixture was condensed under reduced pressure. Ether was added to the residue. The generated insoluble matter was separated by filtration and dried to give the title compound (0.32 g) as a white powder.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08822453B2
Quelldatensatzuspto-grants-2014_09
ORD IDord-de8ab4288e134fb39d21852ded4f2ecc
Quellennotizuspto-grants-2014_09