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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 2089631Erstellt: 26. Oktober 2026

Dimethylformamide → HCID 68212999, Verbindung

https://huagongshe.com/reaction/2089631

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktDimethylformamideHCID 6228—
EduktCesium carbonateHCID 10796—
Edukt3-Methoxy-2,2-dimethylpropionic acid chloromethyl esterHCID 14459693—
EduktN-[1-amino-1-(4-{[[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}phenyl)methylidene]benzamideHCID 136334022—
LösungsmittelWaterHCID 962—
LösungsmittelEthyl AcetateHCID 8857—
ProduktHCID 68212999HCID 6821299935,8%

Reaktionsbedingungen

Temperatur60 °C

Reaktionsschritte

To a mixture of N-[1-amino-1-(4-{[[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}phenyl)methylidene]benzamide (Example 1a, 45 mg) and DMF (2 mL), cesium carbonate (29 mg) and 3-methoxy-2,2-dimethylpropionic acid chloromethyl ester (20 mg) were sequentially added, and the resulting mixture was stirred at 60° C. for 4 hours. The resulting mixture was poured into ethyl acetate (30 mL) and water (20 mL). After shaking the mixture, the organic layer was collected. The organic layer was sequentially washed twice with water (30 mL) and with saturated aqueous sodium chloride solution (20 mL), and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain the captioned compound (20 mg).

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08436009B2
Quelldatensatzuspto-grants-2013_05
ORD IDord-527ceb6ba360489dacf24700108e7804
Quellennotizuspto-grants-2013_05